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  1. Attracting, Preparing, and Retaining Under-Represented Populations in Rural and Remote Alberta-North Communities

    Directory of Open Access Journals (Sweden)

    Nancy Steel

    2011-05-01

    Full Text Available For several years, the government of the western Canadian province of Alberta has drafted policies and conducted research on the problem of populations under-represented in adult education. This Alberta-North and Athabasca University study, funded by the Alberta government’s Innovation Fund, uses the advice and educational experiences of northern former and present students, and of other community members, to identify ways of better attracting, preparing, and retaining under-represented populations in northern Alberta communities through provision and training in the use of distance delivery methods.The research reported here commences with a review of the literature to investigate the following: 1 the contribution distance education makes globally to learning access in remote areas (and resulting economic growth for under-served populations; 2 how support is provided to retain isolated students; and 3 the help needed to assist remote students to complete distance programs. Community consultations with social service and education agencies in three communities were conducted in order to obtain their perspectives about what helps to attract and support students to educational programs and the barriers students typically encounter, which might be mitigated by distance methods. Finally, a survey was designed and distributed in 87 Alberta-North communities in northern Alberta and across Canada’s Northwest Territories to add perspective to the consultation results.

  2. Cd4Cu7As, the first representative of a fully ordered, orthorhombically distorted MgCu2 Laves phase.

    Science.gov (United States)

    Osters, Oliver; Nilges, Tom; Schöneich, Michael; Schmidt, Peer; Rothballer, Jan; Pielnhofer, Florian; Weihrich, Richard

    2012-08-06

    The ternary Laves phase Cd(4)Cu(7)As is the first intermetallic compound in the system Cu-Cd-As and a representative of a new substitution variant for Laves phases. It crystallizes orthorhombically in the space group Pnnm (No. 58) with lattice parameters a = 9.8833(7) Å; b = 7.1251(3) Å; c = 5.0895(4) Å. All sites are fully occupied within the standard deviations. The structure can be described as typical Laves phase, where Cu and As are forming vertex-linked tetrahedra and Cd adopts the structure motive of a distorted diamond network. Cd(4)Cu(7)As was prepared from stoichiometric mixtures of the elements in a solid state reaction at 1000 °C. Magnetic measurements are showing a Pauli paramagnetic behavior. During our systematical investigations within the ternary phase triangle Cd-Cu-As the cubic C15-type Laves phase Cd(4)Cu(6.9(1))As(1.1(1)) was structurally characterized. It crystallizes cubic in the space group Fd3m with lattice parameter a = 7.0779(8) Å. Typically for quasi-binary Laves phases Cu and As are both occupying the 16c site. Chemical bonding, charge transfer and atomic properties of Cd(4)Cu(7)As were analyzed by band structure, ELF, and AIM calculations. On the basis of the general formula for Laves phases AB(2), Cd is slightly positively charged forming the A substructure, whereas Cu and As represent the negatively charged B substructure in both cases. The crystal structure distortion is thus related to local effects caused by Arsenic that exhibits a larger atomic volume (18 Å(3) compared to 13 Å(3) for Cu) and higher ionicity in bonding.

  3. Efficient Preparation of Metal Organosols by Phase Transfer

    Institute of Scientific and Technical Information of China (English)

    ZHAO Ji-Kuan; CHEN Xiao; YANG Chun-Jie; SUI Zhen-Ming; ZHANG Guo-Dong; CHAI Yong-Cun; LIU Jie

    2005-01-01

    Organosols of silver and gold nanoparticles stabilized by sodium oleate were prepared with high efficiency by simple phase transfer of their hydrosols to isooctane. Concentrations of sodium oleate and magnesium chloride have crucial effects on the phase transfer efficiency. UV-visible absorption spectroscopy and transmission electron microscopy have been used to characterize the nanoparticles. A possible phase transfer mechanism was proposed based on the anchoring positions of oleate deduced by molecular modeling calculations.

  4. Phase 1 Front-End CMS Calorimeter (HE) Upgrade Preparation

    CERN Document Server

    Bunin, Pavel

    2016-01-01

    Preparation of HE Phase 1 Front-End upgrade is shown. For the final quality control of the new generation HE front-end electronics components a Burn-in stand has been prepared. All electronics components are being tested on the burn-in stand and should pass through the burn-in QC before the installation on the CMS. First tests and results are presented.

  5. The majority of patients with metastatic melanoma are not represented in pivotal phase III immunotherapy trials

    DEFF Research Database (Denmark)

    Donia, Marco; Kimper-Karl, Marie Louise; Høyer, Katrine Lundby

    2017-01-01

    in 2014, were included in the analysis. Seven pre-defined eligibility criteria, all used to select patients for enrolment in five recent randomised phase III immunotherapy trials, were analysed. Results Fifty-five percent of the total population with MM did not meet one or more eligibility criteria (‘not...... worse baseline prognostic features. However, patients treated with immunotherapy had similar survival outcomes regardless of eligibility. Conclusion Over half of the patients evaluated for systemic treatment of MM are not represented in phase III registration immunotherapy trials. The data reveal a huge...... knowledge gap regarding the usefulness of new immunotherapies in the ‘real-world’ patient population, and urge additional testing of known regimens in selected poor prognosis cohorts....

  6. Attracting, Preparing, and Retaining Under-Represented Populations in Rural and Remote Alberta-North Communities

    Science.gov (United States)

    Steel, Nancy; Fahy, Patrick J.

    2011-01-01

    For several years, the government of the western Canadian province of Alberta has drafted policies and conducted research on the problem of populations under-represented in adult education. This Alberta-North and Athabasca University study, funded by the Alberta government's Innovation Fund, uses the advice and educational experiences of northern…

  7. Preparation, physical property and thermal physical property of phase change microcapsule slurry and phase change emulsion

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Rui [Department of Chemical Engineering, Tsinghua University, Beijing 100084 (China); Xu, Hui; Zhang, Yingping [School of Architecture, Tsinghua University, Beijing 100084 (China)

    2003-12-01

    Phase change microcapsule slurry and phase change emulsion are two novel two-phase heat transfer fluids. Compared with a conventional single-phase heat transfer fluid such as water, their apparent specific heats in the phase change temperature range are greatly increased. Due to this, the heat transfer ability and energy transport ability can be obviously improved. Therefore, they have many potentially important applications in fields such as heating, ventilating, air-conditioning, refrigeration and heat exchangers. In this paper, a phase change emulsion was prepared by mixing film synthesis, and a phase change microcapsule slurry was prepared by in situ polymerization with polystyrene, polymethyl methacrylate, polyethyl methacrylate as encapsulation material, respectively. Physical properties, such as viscosity, diameter and its distribution of microcapsule and emulsion were investigated. The relationship between the concentration of tetradecane and physical properties have been discussed in detail. Meanwhile, the thermal physical properties of these two fluids were determined by DSC. Also, the influence of tetradecane concentration on phase change temperature and phase change heat has been discussed.

  8. Preparation, physical property and thermal physical property of phase change microcapsule slurry and phase change emulsion

    Energy Technology Data Exchange (ETDEWEB)

    Rui Yang [Tsinghua Univ., Dept. of Chemical Engineering, Beijing (China); Hui Xu; Yingping Zhang [Tsinghua Univ., School of Architecture, Beijing (China)

    2003-12-01

    Phase change microcapsule slurry and phase change emulsion are two novel two-phase heat transfer fluids. Compared with a conventional single-phase heat transfer fluid such as water, their apparent specific heats in the phase change temperature range are greatly increased. Due to this, the heat transfer ability and energy transport ability can be obviously improved. Therefore, they have many potentially important applications in fields such as heating, ventilating, air-conditioning, refrigeration and heat exchangers. In this paper, a phase change emulsion was prepared by mixing film synthesis, and a phase change microcapsule slurry was prepared by in situ polymerization with polystyrene, polymethyl methacrylate, polyethyl methacrylate as encapsulation material, respectively. Physical properties, such as viscosity, diameter and its distribution of microcapsule and emulsion were investigated. The relationship between the concentration of tetradecane and physical properties have been discussed in detail. Meanwhile, the thermal physical properties of these two fluids were determined by DSC. Also, the influence of tetradecane concentration on phase change temperature and phase change heat has been discussed. (Author)

  9. Preparation of Phase Change Microcapsule and Its Plication in Textiles

    Institute of Scientific and Technical Information of China (English)

    MIN Jie; SHOU Chen-yan

    2010-01-01

    Phase change microcapsules(PCMs)are prepared with n-hexadecane and n-octadecane as core material,and melamine-formaldehyde resin is used as shell material by in-situ polymerization.Differential scanning calorimetry (DSC) was used to analyze the phase change properties.Thermal conductivity and maximum heat flux of cotton fabric finished with PCMs before and after being washed were also measured.It has been found that melting and crystal enthalpy of the PCMs decrease with decreasing the core/shell ratio,while q_max of fabric treated with PCMs decreases and the thermal conductivity increases.Study shows that fabric finished by the PCMS has good temperature conditioning function.

  10. A Simple and Rapid Method for Standard Preparation of Gas Phase Extract of Cigarette Smoke

    Science.gov (United States)

    Higashi, Tsunehito; Mai, Yosuke; Noya, Yoichi; Horinouchi, Takahiro; Terada, Koji; Hoshi, Akimasa; Nepal, Prabha; Harada, Takuya; Horiguchi, Mika; Hatate, Chizuru; Kuge, Yuji; Miwa, Soichi

    2014-01-01

    Cigarette smoke consists of tar and gas phase: the latter is toxicologically important because it can pass through lung alveolar epithelium to enter the circulation. Here we attempt to establish a standard method for preparation of gas phase extract of cigarette smoke (CSE). CSE was prepared by continuously sucking cigarette smoke through a Cambridge filter to remove tar, followed by bubbling it into phosphate-buffered saline (PBS). An increase in dry weight of the filter was defined as tar weight. Characteristically, concentrations of CSEs were represented as virtual tar concentrations, assuming that tar on the filter was dissolved in PBS. CSEs prepared from smaller numbers of cigarettes (original tar concentrations ≤15 mg/ml) showed similar concentration-response curves for cytotoxicity versus virtual tar concentrations, but with CSEs from larger numbers (tar ≥20 mg/ml), the curves were shifted rightward. Accordingly, the cytotoxic activity was detected in PBS of the second reservoir downstream of the first one with larger numbers of cigarettes. CSEs prepared from various cigarette brands showed comparable concentration-response curves for cytotoxicity. Two types of CSEs prepared by continuous and puff smoking protocols were similar regarding concentration-response curves for cytotoxicity, pharmacology of their cytotoxicity, and concentrations of cytotoxic compounds. These data show that concentrations of CSEs expressed by virtual tar concentrations can be a reference value to normalize their cytotoxicity, irrespective of numbers of combusted cigarettes, cigarette brands and smoking protocols, if original tar concentrations are ≤15 mg/ml. PMID:25229830

  11. In vivo measurement of dynamic rectus femoris function at postures representative of early swing phase.

    Science.gov (United States)

    Hernández, Antonio; Dhaher, Yasin; Thelen, Darryl G

    2008-01-01

    Forward dynamic models suggest that muscle-induced joint motions depend on dynamic coupling between body segments. As a result, biarticular muscles may exhibit non-intuitive behavior in which the induced joint motion is opposite to that assumed based on anatomy. Empirical validation of such predictions is important for models to be relied upon to characterize muscle function. In this study, we measured, in vivo, the hip and knee accelerations induced by electrical stimulation of the rectus femoris (RF) and the vastus medialis (VM) at postures representatives of the toe-off and early swing phases of the gait cycle. Seven healthy young subjects were positioned side-lying with their lower limb supported on air bearings while a 90 ms pulse train stimulated each muscle separately or simultaneously. Lower limb kinematics were measured and compared to predictions from a similarly configured dynamic model of the lower limb. We found that both RF and VM, when stimulated independently, accelerated the hip and knee into extension at these postures, consistent with model predictions. Predicted ratios of hip acceleration to knee acceleration were generally within 1 s.d. of average values. In addition, measured responses to simultaneous RF and VM stimulation were within 13% of predictions based on the assumption that joint accelerations induced by activating two muscles simultaneously can be found by adding the joint accelerations induced by activating the same muscles independently. These results provide empirical evidence of the importance of considering dynamic effects when interpreting the role of muscles in generating movement.

  12. Solid-Phase Preparation and Characterization of Chitosan

    Institute of Scientific and Technical Information of China (English)

    GaoLe-ping; DuYu-min; ZhangDao-bin; ShiXiao-wen; ZhanHuai-yu; SongWen-hua

    2003-01-01

    Chitosan was prepared with stressing method by blending chitin and solid alkali in a single-screw extruder at given temperature and characterized by potentiometric titration, gel permeation chromatography (GPC), infrared spectrum (IR) and carborr13 magnetic resonance sperctroscopy (13C NMR). Chitosan with a deacetylation degree (DD) of 76. 1% was obtained at a mass ratio 0.2 : 1 : 1 for H20/chitin/NaOH at 160℃ for 12 mirL Compared to conventional solution method(usually 1 : 10 for chitin/NaOH), the alkali assumption greatly decreased. Molecular weight of chitosan obtained by solid-phase method(S3,M. 1.54 X 10s ) was lower than that obtained by suspension method(Y2,Mw3. 34×105). During deacetylation, molecular weight decreased with high reaction temperature and long reaction time but remained same at different initial ratios of NaOH/chitirL It might be concluded that degradation of chitosan was caused by breakout of the main chain of the oxidized chitosan catalyzed by alkali during the deactylation. IR and 13C NMR showed that structures of chitosans prepared by solid-phase method were not changed.

  13. The Cell Cycle: An Activity Using Paper Plates to Represent Time Spent in Phases of the Cell Cycle

    Science.gov (United States)

    Scherer, Yvette D.

    2014-01-01

    In this activity, students are given the opportunity to combine skills in math and geometry for a biology lesson in the cell cycle. Students utilize the data they collect and analyze from an online onion-root-tip activity to create a paper-plate time clock representing a 24-hour cell cycle. By dividing the paper plate into appropriate phases of…

  14. The Cell Cycle: An Activity Using Paper Plates to Represent Time Spent in Phases of the Cell Cycle

    Science.gov (United States)

    Scherer, Yvette D.

    2014-01-01

    In this activity, students are given the opportunity to combine skills in math and geometry for a biology lesson in the cell cycle. Students utilize the data they collect and analyze from an online onion-root-tip activity to create a paper-plate time clock representing a 24-hour cell cycle. By dividing the paper plate into appropriate phases of…

  15. Preparation and application of reversed phase chromatorotor for the isolation of natural products by centrifugal preparative chromatography

    Science.gov (United States)

    A method of preparation of Chromatorotor or plates with a reversed phase (RP) solid silica gel sorbent layer has been developed for preparative centrifugal chromatography. The RP-rotor plates consist of binder free RP solid SiO2 sorbent layers of different thicknesses paked between two supported cir...

  16. A Local Condensation Analysis Representing Two-phase Annular Flow in Condenser/radiator Capillary Tubes

    Science.gov (United States)

    Karimi, Amir

    1991-01-01

    NASA's effort for the thermal environmental control of the Space Station Freedom is directed towards the design, analysis, and development of an Active Thermal Control System (ATCS). A two phase, flow through condenser/radiator concept was baselined, as a part of the ATCS, for the radiation of space station thermal load into space. The proposed condenser rejects heat through direct condensation of ATCS working fluid (ammonia) in the small diameter radiator tubes. Analysis of the condensation process and design of condenser tubes are based on the available two phase flow models for the prediction of flow regimes, heat transfer, and pressure drops. The prediction formulas use the existing empirical relationships of friction factor at gas-liquid interface. An attempt is made to study the stability of interfacial waves in two phase annular flow. The formulation is presented of a stability problem in cylindrical coordinates. The contribution of fluid viscosity, surface tension, and transverse radius of curvature to the interfacial surface is included. A solution is obtained for Kelvin-Helmholtz instability problem which can be used to determine the critical and most dangerous wavelengths for interfacial waves.

  17. Phase analysis of aluminium modified GeSbTe bulk prepared from XRD of samples

    Science.gov (United States)

    Sandhu, Sharanjit; Singh, D.; Kumar, S.; Thangaraj, R.

    2016-05-01

    Various compositions of Aluminium modified GST as Alx(Ge2Sb2Te5)1-x x= 0, 0.15, 0.20, 0.25, 0.30 are prepared to study as a phase change material. Bulk prepared is studied with XRD scans for various phases formed. Phases other than Ge2Sb2Te5 do come in but dominated one is Ge2Sb2Te5 hexagonal phase.

  18. Preparation of Pt/C Catalyst with Solid Phase Reaction Method

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The Pt/C catalyst was prepared with solid phase reaction method (Pt/C(S)) for the first time. Its performances were compared with that prepared by the traditional liquid phase reaction method. The results demonstrate that the electrocatalytic activity of Pt/C catalyst with solid phase reaction method for methanol oxidation is higher than that with liquid phase reaction method. XRD and TEM measurements indicate that the Pt/C(S) possesses low crystalline extent and small particle size.

  19. Analysis of phase error effects in multishot diffusion-prepared turbo spin echo imaging.

    Science.gov (United States)

    Van, Anh T; Cervantes, Barbara; Kooijman, Hendrik; Karampinos, Dimitrios C

    2017-04-01

    To characterize the effect of phase errors on the magnitude and the phase of the diffusion-weighted (DW) signal acquired with diffusion-prepared turbo spin echo (dprep-TSE) sequences. Motion and eddy currents were identified as the main sources of phase errors. An analytical expression for the effect of phase errors on the acquired signal was derived and verified using Bloch simulations, phantom, and in vivo experiments. Simulations and experiments showed that phase errors during the diffusion preparation cause both magnitude and phase modulation on the acquired data. When motion-induced phase error (MiPe) is accounted for (e.g., with motion-compensated diffusion encoding), the signal magnitude modulation due to the leftover eddy-current-induced phase error cannot be eliminated by the conventional phase cycling and sum-of-squares (SOS) method. By employing magnitude stabilizers, the phase-error-induced magnitude modulation, regardless of its cause, was removed but the phase modulation remained. The in vivo comparison between pulsed gradient and flow-compensated diffusion preparations showed that MiPe needed to be addressed in multi-shot dprep-TSE acquisitions employing magnitude stabilizers. A comprehensive analysis of phase errors in dprep-TSE sequences showed that magnitude stabilizers are mandatory in removing the phase error induced magnitude modulation. Additionally, when multi-shot dprep-TSE is employed the inconsistent signal phase modulation across shots has to be resolved before shot-combination is performed.

  20. Robust Multiscale Modelling Of Two-Phase Steels On Heterogeneous Hardware Infrastructures By Using Statistically Similar Representative Volume Element

    Directory of Open Access Journals (Sweden)

    Rauch Ł.

    2015-09-01

    Full Text Available The coupled finite element multiscale simulations (FE2 require costly numerical procedures in both macro and micro scales. Attempts to improve numerical efficiency are focused mainly on two areas of development, i.e. parallelization/distribution of numerical procedures and simplification of virtual material representation. One of the representatives of both mentioned areas is the idea of Statistically Similar Representative Volume Element (SSRVE. It aims at the reduction of the number of finite elements in micro scale as well as at parallelization of the calculations in micro scale which can be performed without barriers. The simplification of computational domain is realized by transformation of sophisticated images of material microstructure into artificially created simple objects being characterized by similar features as their original equivalents. In existing solutions for two-phase steels SSRVE is created on the basis of the analysis of shape coefficients of hard phase in real microstructure and searching for a representative simple structure with similar shape coefficients. Optimization techniques were used to solve this task. In the present paper local strains and stresses are added to the cost function in optimization. Various forms of the objective function composed of different elements were investigated and used in the optimization procedure for the creation of the final SSRVE. The results are compared as far as the efficiency of the procedure and uniqueness of the solution are considered. The best objective function composed of shape coefficients, as well as of strains and stresses, was proposed. Examples of SSRVEs determined for the investigated two-phase steel using that objective function are demonstrated in the paper. Each step of SSRVE creation is investigated from computational efficiency point of view. The proposition of implementation of the whole computational procedure on modern High Performance Computing (HPC

  1. Preparation of Firefighting Hood for Cooling for Phase Change Materials

    Directory of Open Access Journals (Sweden)

    Shu Hwa Lin

    2016-10-01

    Full Text Available There are two types of Phase Change Materials (PCMs which have been developed and adopted in textiles: heat (energy released and cool (energy absorbed. This paper discusses current PCM applications and explores future applications in firefighting gear. Phase change materials are considered latent heat storage units because as they change phase from solid to liquid, liquid to gas and vice versa, energy in the form of heat is absorbed or released. The goal of PCM textiles is to create reusable energy to maintain body temperature, as well as to optimize the performance of protective wear such as hoods. When the wearer’s body temperature increases or decreases, the PCMs applied to the fabric will change state helping to regulate the wearer’s body temperature by providing warmth or cooling. Maintaining a stable body temperature can improve working conditions and comfort.

  2. Preparation of Firefighting Hood for Cooling For Phase Change Materials

    Directory of Open Access Journals (Sweden)

    Shu Hwa Lin

    2016-10-01

    Full Text Available There are two types of Phase Change Materials (PCMs which have been developed and adopted in textiles: heat (energy released and cool (energy absorbed. This paper discusses current PCM applications and explores future applications in firefighting gear. Phase change materials are considered latent heat storage units because as they change phase from solid to liquid, liquid to gas and vice versa, energy in the form of heat is absorbed or released. The goal of PCM textiles is to create reusable energy to maintain body temperature, as well as to optimize the performance of protective wear such as hoods. When the wearer’s body temperature increases or decreases, the PCMs applied to the fabric will change state helping to regulate the wearer’s body temperature by providing warmth or cooling. Maintaining a stable body temperature can improve working conditions and comfort.

  3. Preparation and characterization of magnetic phase-change microcapsules

    Institute of Scientific and Technical Information of China (English)

    HUANG Yong; XUAN YiMin; LI Qiang; CHE JianFei

    2009-01-01

    Magnetic microcapsules containing paraffin cores within urea-formaldehyde shells were fabricated utilizing in situ polymerization, with iron nano-particles as magnetic particles. The thermal properties,surface morphologies, magnetic properties and iron nano-particles content of the magnetic phase-change microcapsules were investigated by scanning electronic microscopy (SEM), differential scan-ning calorimetry (DSC), vibrating sample magnetometry (VSM) and inductively coupled plasma quan-tometry (ICP). The influence of iron nano-particles on morphologies was also considered. The results indicate that the melting point of magnetic phase-change microcapsules is almost identical to that of paraffin. The magnetism parameters such as specific saturation magnetization and residual magneti-zation of magnetic phase-change microcapsules increase with the increase of iron nano-particles content.

  4. Preparation of Plutonium Counting Source Using Solid Phase Extraction Disk

    Institute of Scientific and Technical Information of China (English)

    SUN; Hong-qing; YANG; Su-liang; DING; You-qian; YANG; Jin-ling; MAO; Guo-shu

    2013-01-01

    For the determination of trace amount of plutonium,Pu(Ⅳ)may be extracted from dilute nitric acid by TTA-xylene,and stripped by concentrated nitric acid.But the small volume of strip solution used in traditional counting source preparation by direct evaporation could lead to a rather high detection limit.Plutonium in strip solution may all be absorbed on the surface of an anion exchange resin disk.And

  5. PREPARATION OF WATERBORNE ULTRAFINE PARTICLES OF EPOXY RESIN BY PHASE INVERSION TECHNIQUE

    Institute of Scientific and Technical Information of China (English)

    YANG Zhengzhong; XU Yuanze; WANG Shengjie; YU Hao; CAI Weizhen

    1997-01-01

    Waterborne ultrafine particles of epoxy resin were prepared by phase inversion technique The results of SEM revealed that the particles diameter was in the range of 50 to l()am and the effects on amount of water required at phase inversion point were also dis()ed.

  6. Preparation of ITO Nanoparticles by Liquid Phase Coprecipitation Method

    Directory of Open Access Journals (Sweden)

    Zhanlai Ding

    2010-01-01

    Full Text Available The nanoscale indium tin oxide (ITO particles are synthesied by liquid phase coprecipitation method under given conditions with solution of indium chloride, tin chloride, and ammonia. The absolute ethyl alcohol or deionized water was used as solvent and the dodecylamine or hexadecylamine surfactant was used as a dispersant in the reaction system. The sample powder was characterized by X-ray diffraction (XRD, transmission electron microscopy (TEM, and high-resolution electron microscopy (HRTEM. Based on the transmission electron micrograph, the influences of the two different solvents and the two different dispersants on the nanoparticle size and dispersion were studied, respectively. The results showed that the ITO particles are finely crystallized body-centered cubic structure. The particle size has distributed in 30 nm to 90 nm.

  7. Low-Order GAM Admire System in Landing Preparation Phase

    Directory of Open Access Journals (Sweden)

    Ionel IORGA

    2011-09-01

    Full Text Available In this paper the symbolic and numeric computations for the simplified GAM (Generic Aerodynamic Model Admire system are presented . The numeric computations were performed into the MatLab environment with the aim of presenting to the reader the details of the preparation for landing of the airplane generic model. Regarding the symbolic computations that have been made it's worth to mention here the fact that they concerned the issues of stability in the manner that the trim point for the low order non-linear system was computed and an analysis of the eigenvalues of the Jacobian matrix associated to the system, which has been evaluated in the trim point, was performed. The case of the stable longitudinal level descending flight and the case of transition to a state appropriate for the touch-down are presented. It is shown the fact that the plane can regain stability if the real moment for touch-down is missed by reentering into the stable longitudinal level descending flight (by usage of the control e.

  8. Electromembrane extraction--three-phase electrophoresis for future preparative applications.

    Science.gov (United States)

    Gjelstad, Astrid; Pedersen-Bjergaard, Stig

    2014-09-01

    The purpose of this article is to discuss the principle and the future potential for electromembrane extraction (EME). EME was presented in 2006 as a totally new sample preparation technique for ionized target analytes, based on electrokinetic migration across a supported liquid membrane under the influence of an external electrical field. The principle of EME is presented, and typical performance data for EME are discussed. Most work with EME up to date has been performed with low-molecular weight pharmaceutical substances as model analytes, but the principles of EME should be developed in other directions in the future to fully explore the potential. Recent research in new directions is critically reviewed, with focus on extraction of different types of chemical and biochemical substances, new separation possibilities, new approaches, and challenges related to mass transfer and background current. The intention of this critical review is to give a flavor of EME and to stimulate into more research in the area of EME. Unlike other review articles, the current one is less comprehensive, but put more emphasis on new directions for EME.

  9. Effect of annealing on phase transition in poly(vinylidene fluoride) films prepared using polar solvent

    Indian Academy of Sciences (India)

    S Satapathy; Santosh Pawar; P K Gupta; K B R Varma

    2011-07-01

    The -phase poly (vinylidene fluoride) (PVDF) films are usually prepared using dimethyl sulfoxide (DMSO) solvent, regardless of preparation temperature. Here we report the crystallization of both and -phase PVDF films by varying preparation temperature using DMSO solvent. The -phase PVDF films were annealed at 70, 90, 110, 130 and 160°C for five hours. The changes in the phase contents in the PVDF at different annealing conditions have been described. When thin films were annealed at 90°C for 5 h, maximum percentage of -phase appears in PVDF thin films. The -phase PVDF films completely converted to -phase when they were annealed at 160°C for 5 h. From X-ray diffraction (XRD), Fourier transform infrared spectrum (FTIR), differential scanning calorimetry (DSC) and Raman studies, it is confirmed that the PVDF thin films, cast from solution and annealed at 90°C for 5 h, have maximum percentage of -phase. The -phase PVDF shows a remnant polarization of 4.9 C/cm2 at 1400 kV/cm at 1 Hz.

  10. HiLumi prepares its construction phase with industry

    CERN Multimedia

    Agnes Szeberenyi

    2015-01-01

    The High-Luminosity LHC project is now seeking industrial suppliers and collaborations to start the construction phase and make the high-luminosity upgrade happen. The “HiLumi LHC goes to Industry” event held on 26 June aimed to foster R&D collaborations and knowledge exchange between CERN and small and medium-sized enterprises (SMEs) - the perfect opportunity for them to match their capacity with the requirements of HiLumi.   Isabel Bejar-Alonso (High-Luminosity LHC Technical Coordinator) addresses the participants of the “HiLumi LHC goes to Industry” event held at IdeaSquare on 26 June. To reach the 14 TeV and 3000 fb-1 goal of the High-Luminosity LHC, more than 1.2 km of the current LHC machine will need to be replaced with high-technology components that require cutting-edge technologies. HiLumi experts have already identified more than 65 technology areas and even more challenging components that need to be manufactured, assembled and tested bef...

  11. PREPARATION OF BISPHENOL A EPOXY RESIN WATERBORNE DISPERSIONS BY THE PHASE INVERSION EMULSIFICATION TECHNIQUE

    Institute of Scientific and Technical Information of China (English)

    Zhen-zhong Yang; De-lu Zhao

    2000-01-01

    The phase inversion emulsification technique (PIET) is an effective physical method for preparing waterborne dispersions of polymer resins. Some results concerning the preparation of bisphenol A epoxy resin waterborne dispersions by PIET in our laboratory were summarized. Electrical properties, rheological behavior and morphological evolution during phase inversion progress were systematically characterized. The effects of the emulsifier concentration and emulsification temperature on phase inversion progress and the structural features of the waterborne particles were studied as well. The deformation and break up of water drops in a shear field were analyzed in terms of micro-rheology, while the interaction and coalescence dynamics of water drops were discussed in terms of DLVO theory and Smoluchowski effective collision theory,respectively. Based on the experimental results and theoretical analysis, a physical model of phase inversion progress was suggested, by which the effects of the parameters on phase inversion progress and the structural features of the waterborne particles were interpreted and predicted.

  12. Jules Horowitz Reactor: Organisation for the Preparation of the Commissioning Phase and Normal Operation

    Energy Technology Data Exchange (ETDEWEB)

    Estrade, J.; Fabre, J. L.; Marcille, O. [French Alternative Energies end Atomic Energy Commission, Provence (France)

    2013-07-01

    The Jules Horowitz Reactor (JHR) is a new modern Material Testing Reactor (MTR) currently under construction at CEA Cadarache research centre in the south of France. It will be a major research facility in support to the development and the qualification of materials and fuels under irradiation with sizes and environment conditions relevant for nuclear power plants in order to optimise and demonstrate safe operations of existing power reactors as well as to support future reactors design. It will represent also an important research infrastructure for scientific studies dealing with material and fuel behaviour under irradiation. The JHR will contribute also to secure the production of radioisotope for medical application. This is a key public health stake. The construction of JHR which started in 2007 is going-on with target of commissioning by the end of 2017. The design of the reactor provides modern experimental capacity in support to R and D programs for the nuclear energy for the next 60 years. In parallel to the facility construction, the preparation of the future staff and of the organisation to operate the reactor safely, reliably and efficiently is an important issue. In this framework, many actions are in progress to elaborate: Ο the staffing and the organisational structure for the commissioning test phases and also for normal operation, Ο the documentation in support to the reactor operation (safety analysis report, general operating rules, procedures, instructions, ···), Ο the maintenance, in service and periodic test programs, Ο staff training programs by using dedicated facilities (simulator, ···) Ο commissioning test programs for ensuring that the layout of systems and subcomponents is completed in accordance with the design requirements, the specification performances and the safety criteria. These commissioning tests will also be helpful for transferring the knowledge on the installed systems to the operating group. This paper gives the

  13. Preparative soft and reactive landing of gas-phase ions on plasma-treated metal surfaces.

    Science.gov (United States)

    Volný, Michael; Elam, W Timothy; Ratner, Buddy D; Turecek, Frantisek

    2005-08-01

    Soft landing of singly charged gas-phase ions on dry metal surfaces that were pretreated in situ by oxygen plasma results in 0.1-2% total yields of recovered intact compounds. Lysine, peptides, crystal violet dye, and a biotin conjugate are found to survive soft landing of hyperthermal ions of up to 50-eV kinetic energy. Soft landing at 40-50-eV ion kinetic energies of a fluorescence-labeled biotin conjugate results in an immobilized fraction that cannot be washed from the surface and is found to contain an intact biotin moiety. The present results represent an approximately 10(4) fold improvement in soft-landing efficiency and indicate that plasma-treated metal surfaces can be useful for preparative separation of organic and biological molecules by mass spectrometry. The substantial improvement in soft-landing yields results from a high transmission of electrosprayed ions into the vacuum system, efficient and nondestructive discharge of ions on the metal oxide surface, and facile analyte recovery in the absence of a matrix.

  14. Preparation and Evaluation of Immobilized SE-30 Coated Stationary Phases for CEC

    Institute of Scientific and Technical Information of China (English)

    NingBaoming; ZhengJie; ZhangGuodong; XuBingjiu

    2001-01-01

    A new type of stationary phase for capillary electrochromatography (CEC), immobilized SE-30 coated silica gel, was developed and the columns packed with this new phase were prepared and evaluated. It was found that this phase could be used to make frits for the micro-columns as well as to pack the bulk of the column. By sticking together the particles in the whole of the column bed, this new packing resulted in columns with stable performance, even under rigorous conditions: more than 380 consecutive separations were effected with these columns with the mobile phase pH of 11.7.

  15. Lag phase is a distinct growth phase that prepares bacteria for exponential growth and involves transient metal accumulation.

    Science.gov (United States)

    Rolfe, Matthew D; Rice, Christopher J; Lucchini, Sacha; Pin, Carmen; Thompson, Arthur; Cameron, Andrew D S; Alston, Mark; Stringer, Michael F; Betts, Roy P; Baranyi, József; Peck, Michael W; Hinton, Jay C D

    2012-02-01

    Lag phase represents the earliest and most poorly understood stage of the bacterial growth cycle. We developed a reproducible experimental system and conducted functional genomic and physiological analyses of a 2-h lag phase in Salmonella enterica serovar Typhimurium. Adaptation began within 4 min of inoculation into fresh LB medium with the transient expression of genes involved in phosphate uptake. The main lag-phase transcriptional program initiated at 20 min with the upregulation of 945 genes encoding processes such as transcription, translation, iron-sulfur protein assembly, nucleotide metabolism, LPS biosynthesis, and aerobic respiration. ChIP-chip revealed that RNA polymerase was not "poised" upstream of the bacterial genes that are rapidly induced at the beginning of lag phase, suggesting a mechanism that involves de novo partitioning of RNA polymerase to transcribe 522 bacterial genes within 4 min of leaving stationary phase. We used inductively coupled plasma mass spectrometry (ICP-MS) to discover that iron, calcium, and manganese are accumulated by S. Typhimurium during lag phase, while levels of cobalt, nickel, and sodium showed distinct growth-phase-specific patterns. The high concentration of iron during lag phase was associated with transient sensitivity to oxidative stress. The study of lag phase promises to identify the physiological and regulatory processes responsible for adaptation to new environments.

  16. Preparation of anatase/rutile mixed-phase titania nanoparticles for dye-sensitized solar cells.

    Science.gov (United States)

    Hwang, Yong-Kyung; Park, Sung Soo; Lim, Jun-Heok; Won, Yong Sun; Huh, Seong

    2013-03-01

    Acid-labile high surface mesoporous ZnO/Zn(OH)2 composite material is used as a novel hard template for the preparation of mesoporous amorphous TiO2. The template-free amorphous TiO2 material is then thermally crystallized at suitable temperature to control the relative ratio of anatase and rutile phases in a particle. Four different anatase/rutile (AR) mixed-phase TiO2 nanoparticles (AR-3, AR-15, AR-20, and AR-23 denoted for the samples of 3%, 15%, 20%, and 23% rutile phase, respectively) are prepared and characterized by powder X-ray diffraction (PXRD) and transmission electron microscopy (TEM). The coexistence of anatase and rutile phases in a TiO2 nanoparticle is visually confirmed by HRTEM analysis. These mixed-phase TiO2 nanoparticles are examined as candidates for photoelectrodes of dye-sensitized solar cells (DSSCs). The J-V curves and IPCE spectra for the DSSCs prepared from the mixed-phase TiO2 nanoparticles are obtained, and their photovoltaic properties are investigated. The photo-conversion efficiency (eta) indicates the highest value of 5.07% for AR-20. The synergistic effect of coexisting anatase and rutile phases with an optimal ratio in a TiO2 nanoparticle of AR-20 for an efficient interfacial transfer of photo-generated electrons is likely to lead to the highest efficiency among the AR-n samples.

  17. An Efficient Route to Prepare Metal Organosols by Phase Transfer Procedure

    Institute of Scientific and Technical Information of China (English)

    Ji Kuan ZHAO; Xiao CHEN; Chun Jie YANG; Zhen Ming SUI; Yong Cun CHAI; Guo Dong ZHANG; Jie LIU

    2005-01-01

    Silver and gold organosols are easily prepared by transferring nanoparticles from aqueous phase into isooctane with high efficiency (>90%). Concentrations of sodium oleate and magnesium chloride have crucial effects on the transfer efficiency. Based on the UV-visible absorption spectra, TEM micrographs of nanoparticles, as well as molecular modeling calculation about the adsorption conformation of sodium oleate molecules, a possible phase transfer mechanism is proposed.

  18. Electrical properties of ZnO varistors prepared by direct mixing of constituent phases

    Directory of Open Access Journals (Sweden)

    Žunić M.

    2006-01-01

    Full Text Available Varistor samples containing different amounts of constituent phases were prepared by direct mixing of constituent phases. Detailed electrical characterization was performed to explain the influence of minor phases (spinel and intergranular phases on overall properties. Characterization included investigation of the non-linear coefficients (α, breakdown electric field (EB, leakage currents (JL, grain boundary barrier hight (ΦB and constant β from current-voltage characteristics, as well as calculation of activation energies for conduction (EA from ac impedance spectroscopy in the temperature interval 30-410°C. Varistors sintered at 1100 °C for 1 h showed pronounced differences in electrical properties depending on relative molar ratios of the phases. Results were discussed in the sense of possible reduction of the content of minor phases in ZnO varistors.

  19. Preparation and evaluation of double-phased mucoadhesive suppositories of lidocaine utilizing Carbopol and white beeswax.

    Science.gov (United States)

    Yahagi, R; Onishi, H; Machida, Y

    1999-08-27

    In an attempt to restrict drug absorption from suppositories to only the lower rectum, mucoadhesive lidocaine (LID) suppositories were prepared using Witepsol H-15 as a base, and Carbopol 934P (CP) and white beeswax (WAX) as additives. CP has a mucoadhesive property and WAX gives the suppositories stiffness. The suppositories containing 10% CP and 20% WAX stayed in the lower recta of rats for at least 2 h. Double-phased suppositories consisting of a front layer containing 10% CP and 20% WAX and a terminal layer containing LID and various amounts of CP were prepared. In vitro release profiles of LID from double-phased suppositories were similar to conventional single-phased suppositories containing CP alone. Values of AUC(0-6 h) and MRT of LID after administration of double-phased suppositories to rabbits were larger than those for single-phased suppositories with or without CP. On the other hand, the initial plasma metabolites concentrations after administration of double-phased suppositories were significantly lower and tended to exhibit delayed T(max) compared to single-phased suppositories. These results suggest that the double-phased mucoadhesive suppositories suppress initial metabolism of LID, and may be useful for improving bioavailabilities of drugs, like LID, which accept first-pass effect considerably.

  20. Preparing poly (caprolactone) micro-particles through solvent-induced phase separation

    DEFF Research Database (Denmark)

    Li, Xiaoqiang; Kanjwal, Muzafar Ahmed; Stephansen, Karen

    2012-01-01

    Poly (caprolactone) (PCL) particles with the size distribution from 1 to 100 μm were prepared through solvent-induced phase separation, in which polyvinyl-alcohol (PVA) was used as the matrix-forming polymer to stabilize PCL particles. The cloud point data of PCL-acetone-water was determined...

  1. Membranes Prepared by Self-assembly and Chelation Assisted Phase Inversion

    KAUST Repository

    Xie, Yihui

    2017-05-19

    We combine self-assembly in solution, complexation with metallic salts and phase separation induced by solvent-non-solvent exchange to prepare nanostructured membranes for separation in the nanofiltration range. The method was applied to synthesized poly(acrylic acid)-b-polysulfone-b-poly(acrylic acid) copolymers dissolved in a selective solvent mixture and immersed in aqueous Cu2+ or Ag+ solutions.

  2. The Preparation and Characterization of INTEC Phase 2b Composition Variation Study Glasses

    Energy Technology Data Exchange (ETDEWEB)

    B. A. Staples; B. A. Scholes; L. L. Torres; C. A. Musick; B. R. Boyle (INEEL); D. K. Peeler (SRTC); J. D. Vienna (PNNL)

    2000-02-01

    The second phase of the composition variation study (CVS) for the development of glass compositions to immobilize Idaho Nuclear Technology and Engineering Center (INTEC) high level wastes (HLW) is complete. This phase of the CVS addressed waste composition of high activity waste fractions (HAW) from the initial separations flowsheet. Updated estimates if INTEC calcined HLW compositions and of high activity waste fractions proposed to be separated from dissolved calcine were used as the waste component for this CVS phase. These wastes are of particular interest because high aluminum, calcium, zirconium, fluorine, potassium, and low iron and sodium content places them outside the vitrification experience in the Department of Energy complex. Because of the presence of calcium and fluorine, two major zirconia calcine components not addressed in Phase I, a series of scooping tests, designated Phase 2a, were performed. The results of these tests provided information on the effects of calcium and fluoride solubility and their impacts on product properties and composition boundary information for Phase 2b. Details and results of Phase 2a are reported separately. Through application of statistical techniques and the results of Phase 2a, a test matrix was defined for Phase 2b of the CVS. From this matrix, formulations were systematically selected for preparation and characterization with respect to visual and optical homogeneity, viscosity as a function of melt temperature, liquidus temperature (TL), and leaching properties based on response to the product consistency test. The results of preparing and characterizing the Phase 2b glasses are presented in this document. Based on the results, several formulations investigated have suitable properties for further development. A full analysis of the composition-product characteristic relationship of glasses being developed for immobilizing INTEC wastes will be performed at the completion of composition-property relationship

  3. Vinyl Ester Oligomer Crosslinked Porous Polymers Prepared via Surfactant-Free High Internal Phase Emulsions

    Directory of Open Access Journals (Sweden)

    Yun Zhu

    2012-01-01

    Full Text Available Using vinyl ester resin (VER containing styrene (or methyl methacrylate and vinyl ester oligomer (VEO as external phase, Pickering high internal phase emulsions (Pickering HIPEs having internal phase volume fraction of up to 95 vol% were prepared with copolymer particles as sole stabilizer. Polymerizing the external phase of these Pickering HIPEs led to porous polymers (poly-Pickering-HIPEs. Compared to the polystyrene- (PS- based poly-Pickering-HIPEs which were prepared with mixture of styrene and divinylbenzene (DVB as crosslinker, the poly-Pickering-HIPEs herein showed much higher elastic modulus and toughness. The elastic modulus of these poly-Pickering-HIPEs increased with increasing the VEO concentration in the external phase, while it decreased with increasing internal phase volume fraction. Increasing VEO concentration in the external phase also resulted in a decrease in the average void diameter as well as a narrow void diameter distribution of the resulting poly-Pickering-HIPEs. In addition, there were many small pores in the voids surface caused by the volume contraction of VER during the polymerization, which suggests a new method to fabricate porous polymers having a well-defined hierarchical pore structure.

  4. Nanocasting of Periodic Mesoporous Materials as an Effective Strategy to Prepare Mixed Phases of Titania

    Directory of Open Access Journals (Sweden)

    Luther Mahoney

    2015-12-01

    Full Text Available Mesoporous titanium dioxide materials were prepared using a nanocasting technique involving silica SBA-15 as the hard-template. At an optimal loading of titanium precursor, the hexagonal periodic array of pores in SBA-15 was retained. The phases of titanium dioxide could be easily varied by the number of impregnation cycles and the nature of titanium alkoxide employed. Low number of impregnation cycles produced mixed phases of anatase and TiO2(B. The mesoporous TiO2 materials were tested for solar hydrogen production, and the material consisting of 98% anatase and 2% TiO2(B exhibited the highest yield of hydrogen from the photocatalytic splitting of water. The periodicity of the pores was an important factor that influenced the photocatalytic activity. This study indicates that mixed phases of titania containing ordered array of pores can be prepared by using the nanocasting strategy.

  5. Preparation and Delivery of Protein Microcrystals in Lipidic Cubic Phase for Serial Femtosecond Crystallography.

    Science.gov (United States)

    Ishchenko, Andrii; Cherezov, Vadim; Liu, Wei

    2016-09-20

    Membrane proteins (MPs) are essential components of cellular membranes and primary drug targets. Rational drug design relies on precise structural information, typically obtained by crystallography; however MPs are difficult to crystallize. Recent progress in MP structural determination has benefited greatly from the development of lipidic cubic phase (LCP) crystallization methods, which typically yield well-diffracting, but often small crystals that suffer from radiation damage during traditional crystallographic data collection at synchrotron sources. The development of new-generation X-ray free-electron laser (XFEL) sources that produce extremely bright femtosecond pulses has enabled room temperature data collection from microcrystals with no or negligible radiation damage. Our recent efforts in combining LCP technology with serial femtosecond crystallography (LCP-SFX) have resulted in high-resolution structures of several human G protein-coupled receptors, which represent a notoriously difficult target for structure determination. In the LCP-SFX technique, LCP is recruited as a matrix for both growth and delivery of MP microcrystals to the intersection of the injector stream with an XFEL beam for crystallographic data collection. It has been demonstrated that LCP-SFX can substantially improve the diffraction resolution when only sub-10 µm crystals are available, or when the use of smaller crystals at room temperature can overcome various problems associated with larger cryocooled crystals, such as accumulation of defects, high mosaicity and cryocooling artifacts. Future advancements in X-ray sources and detector technologies should make serial crystallography highly attractive and practicable for implementation not only at XFELs, but also at more accessible synchrotron beamlines. Here we present detailed visual protocols for the preparation, characterization and delivery of microcrystals in LCP for serial crystallography experiments. These protocols include

  6. Preparation of Ion Exchange Films for Solid-Phase Spectrophotometry and Solid-Phase Fluorometry

    Science.gov (United States)

    Hill, Carol M.; Street, Kenneth W.; Tanner, Stephen P.; Philipp, Warren H.

    2000-01-01

    Atomic spectroscopy has dominated the field of trace inorganic analysis because of its high sensitivity and selectivity. The advantages gained by the atomic spectroscopies come with the disadvantage of expensive and often complicated instrumentation. Solid-phase spectroscopy, in which the analyte is preconcentrated on a solid medium followed by conventional spectrophotometry or fluorometry, requires less expensive instrumentation and has considerable sensitivity and selectivity. The sensitivity gains come from preconcentration and the use of chromophore (or fluorophore) developers and the selectivity is achieved by use of ion exchange conditions that favor the analyte in combination with speciative chromophores. Little work has been done to optimize the ion exchange medium (IEM) associated with these techniques. In this report we present a method for making ion exchange polymer films, which considerably simplify the solid-phase spectroscopic techniques. The polymer consists of formaldehyde-crosslinked polyvinyl alcohol with polyacrylic acid entrapped therein. The films are a carboxylate weak cation exchanger in the calcium form. They are mechanically sturdy and optically transparent in the ultraviolet and visible portion of the spectrum, which makes them suitable for spectrophotometry and fluorometry.

  7. Chemical composition of phase I Coxiella burnetii soluble antigen prepared by trichloroacetic acid extraction.

    Science.gov (United States)

    Lukácová, M; Brezina, R; Schramek, S; Pastorek, J

    1989-01-01

    Optimal conditions of extraction (time and temperature) by trichloroacetic acid of soluble antigen from phase I Coxiella burnetii (TCAE), possessing protective properties and used as a chemovaccine against Q fever in men, were studied. Extracts prepared under various conditions were analysed for their polysaccharide, protein and phosphorus contents. Forty-five min of extraction at 0 degrees C were sufficient to obtain a soluble antigen reacting in immunodiffusion with hyperimmune rabbit antiserum. The polysaccharide contents decreased with prolonged extraction at 0 degrees C. At higher extraction temperatures (37 and 100 degrees C), the polysaccharide contents increased while that of proteins decreased. TCAE prepared at 100 degrees C gave no positive immunodiffusion reaction.

  8. A Standardized Method for the Preparation of a Gas Phase Extract of Cigarette Smoke.

    Science.gov (United States)

    Higashi, Tsunehito; Mai, Yosuke; Mazaki, Yuichi; Horinouchi, Takahiro; Miwa, Soichi

    2016-01-01

    The gas phase of cigarette smoke is important from the viewpoint of human health, because it can pass through alveolar epithelium and enter the circulation. There is no standard method for the preparation of a gas phase extract of cigarette smoke (CSE), although CSE is widely used for research instead of whole cigarette smoke. We have established a standard method for the preparation of CSE. One cigarette per trial is continuously combusted under a reduced pressure generated by an aspiration pump with a velocity of 1.050 L/min: the main stream of the smoke is passed through a Cambridge filter to remove tar, and subsequently, bubbled through a glass ball filter (pore size, 20-30 µm) into 15 mL of phosphate-buffered saline (PBS). To express the concentration of CSE, a virtual tar concentration is introduced, which is calculated assuming that tar trapped on the Cambridge filter is dissolved in the PBS. CSEs prepared from smaller numbers of cigarettes (original virtual tar concentration≤15 mg/mL) show similar concentration-response curves for cytotoxicity versus virtual tar concentrations. CSEs prepared from various brands of cigarettes and by different smoking regimes (continuous and puff smoking) show similar cytotoxic potency if the virtual tar concentrations are the same. In conclusion, using the standardized method for CSE preparation in combination with the virtual tar concentration, it becomes possible to simply and rapidly prepare standard CSEs with defined concentrations from any brand of cigarettes, which are toxicologically equivalent to CSE prepared by puff smoking.

  9. PREPARATION OF EVOH MICROPOROUS MEMBRANES via THERMALLY INDUCED PHASE SEPARATION USING BINARY SOLVENTS

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Microporous ethylene-vinyl alcohol copolymer (EVOH) flat membranes and hollow-fiber membranes with 38 mol% ethylene content were prepared via thermally induced phase separation (TIPS) using the mixture of 1,4-butanediol and poly(ethylene glycol)(PEG400) as diluents. Effects of the ratio of 1,4-butanediol to PEG400 on the phase diagrams, phase separation mechanism and membrane morphology were studied by small angle light scattering (SALS) measurements, differential scanning calorimetry (DSC), and scanning electron microscopy (SEM). It was found that by varying the composition of the binary solvent, the phase diagrams and membrane morphology can be controlled successfully. Moreover, the phase diagrams showed that broader regions of Liquid-Liquid (L-L) phase separation were obtained, as well as closer distances between L-L phase separation lines and Solid-Liquid (S-L) phase separation lines. Interconnected structures observed both in the flat membrane and hollow fiber membrane consist with the above results.

  10. Preparing arbitrary pure states of spatial qudits with a single phase-only spatial light modulator

    Science.gov (United States)

    Varga, J. J. M.; Solís-Prosser, A. M. A.; Rebón, L.; Arias, A.; Neves, L.; Iemmi, C.; Ledesma, S.

    2015-04-01

    We present a new method for preparing multidimensional spatial qudits by means of a single phase-only spatial light modulator (SLM). This method improves previous ones that use two SLMs, one working in amplitude regime and the other in phase regime. To that end, we addressed diffraction gratings on the slits that define the state and then we performed a spatial filtering in the Fourier plane. The amplitude of the coefficients of the quantum state are determined by the modulation deep of the diffraction gratings, and the relative phase is the mean phase value of the diffraction gratings. This encoding result to be more compact, less expensive and use the photons more efficiently.

  11. Phase Structural Characteristics of ZrV2 Thin Film Prepared by Magnetron Sputtering

    Institute of Scientific and Technical Information of China (English)

    XU Shi-Lin; SHI Li-Qun

    2005-01-01

    @@ The thin film metal hydride has become an emerging field of research in metal hydride batteries for its good mechanical and hydrogenation properties. ZrV2 thin films have been prepared using a dc magnetron sputtering method, and the phase structure is investigated. Only amorphous or crystalline Zr and V mixture phases are achieved when substrates are heated during either to 400℃ or to 550 ℃. The annealing causes segregation of Zr and V in the film induced by strain-driven diffusion and interdiffusion between substrate Mo and film elements at high temperature, which results in the formation of mixture phases of C14, C15, Zr and V, but the content of C15 phase is not higher compared with that in the bulk material.

  12. The Preparation and Characterization of INTEC HAW Phase I Composition Variation Study Glasses

    Energy Technology Data Exchange (ETDEWEB)

    Musick, C. A.; Peeler, D. K.; Piepel, G. F.; Scholes, B. A.; Staples, B. A.; Vienna, J. D.

    1999-03-01

    A glass composition variation study (CVS) is in progress to define formulations for the vitrification of high activity waste (HAW) proposed to be separated from dissolved calcine stored at the Idaho National Engineering and Environmental Laboratory (INEEL). Estimates of calcine and HAW compositions prepared in FY97 were used to define test matrix glasses. The HAW composition is of particular interest because high aluminum, zirconium, phosphorous and potassium, and low iron and sodium content places it outside the realm of vitrification experience in the Department of Energy (DOE) complex. Through application of statistical techniques, a test matrix was defined for Phase 1 of the CVS. From this matrix, formulations were systematically selected for preparation and characterization with respect to homogeneity, viscosity, liquidus temperature (TL), and leaching response when subjected to the Product Consistency Test (PCT). Based on the properties determined, certain formulations appear suitable for further development including use in planning Phase 2 of the study. It is recommended that glasses to be investigated in Phase 2 be limited to 3-5 wt % phosphate. The results of characterizing the Phase 1 glasses are presented in this document. A full analysis of the composition-property relationships of glasses being developed for immobilizing HAWs will be performing at the completion of CVS phases. This analysis will be needed for the optimization of the glass formulations of vitrifying HAW. Contributions were made to this document by personnel working at the INEEL, Pacific Northwest National Laboratories (PNNL), and the Savannah River Technology Center (SRTC).

  13. Preparation and Characterization of Modified Montmorillonite/Paraffin Phase Change Microcapsules for Energy Storage

    Directory of Open Access Journals (Sweden)

    LIN Sen

    2017-03-01

    Full Text Available The phase change microcapsules of modified montmorillonite/paraffin were prepared by Pickering emulsion method. Analytic techniques of optical microscopy, scanning electron microscopy(SEM, infrared spectroscopy(FTIR, differential scanning calorimetry(DSC and thermogravimetry(TG were utilized for characterizing chemical structure, morphology and thermal properties. Results show that modified montmorillonite as a new type wall material has excellent performance for protecting core material of paraffin. FTIR spectra of phase change of modified montmorillonite/paraffin microcapsules shows that their characteristic peaks match with corresponding peaks of pure paraffin and modified montmorillonite. DSC results indicate that modified montmorillonite/paraffin microcapsules have similar solid-liquid phase change temperature with pure paraffin. The phase transition enthalpy values of microcapsules with paraffin contents varying from 55% to 80% are 110.5-147.2J/g, indicating that microcapsules have excellent thermal storage performance and the phase change properties can be adjusted by changing contents of paraffin. TG results confirm that modified montmorillonite/paraffin microcapsules have outstanding thermal stability. The presented study indicates that modified montmorillonite is a suitable wall material for preparing paraffin microcapsule. Modified montmorillonite/paraffin microcapsules have advantages of low cost and high performance with a great application potential in the field of thermal storage.

  14. Preparation and Characterization of Membranes Formed by Nonsolvent Induced Phase Separation: A Review

    KAUST Repository

    Guillen, Gregory R.

    2011-04-06

    The methods and mechanisms of nonsolvent induced phase separation have been studied for more than fifty years. Today, phase inversion membranes are widely used in numerous chemical industries, biotechnology, and environmental separation processes. The body of knowledge has grown exponentially in the past fifty years, which suggests the need for a critical review of the literature. Here we present a review of nonsolvent induced phase separation membrane preparation and characterization for many commonly used membrane polymers. The key factors in membrane preparation discussed include the solvent type, polymer type and concentration, nonsolvent system type and composition, additives to the polymer solution, and film casting conditions. A brief introduction to membrane characterization is also given, which includes membrane porosity and pore size distribution characterization, membrane physical and chemical properties characterization, and thermodynamic and kinetic evaluation of the phase inversion process. One aim of this review is to lay out the basics for selecting polymer solvent nonsolvent systems with appropriate film casting conditions to produce membranes with the desired performance, morphology, and stability, and to choose the proper way to characterize these properties of nonsolvent induced phase inversion membranes. © 2011 American Chemical Society.

  15. Preparation of novel chiral stationary phase based on click chemistry for ligand exchange chromatography

    Institute of Scientific and Technical Information of China (English)

    Chun Mei Fu; Hong Yu Shi; Guang Sheng Qian; Zhang Wan Li

    2009-01-01

    Click chemistry was applied to immobilize L-proline derivative onto azide-modified silica gel to give a novel chiral stationary phase (denoted as click-CSP) for ligand exchange chromatography. The developed protocol combines the benefits of operational simplicity, exceptionally mild conditions and high surface loadings. The enantioselectivity α of some DE-amino acids on the click-CSP were found to be in the range from 1.13 to 3.46. The chromatographic resolutions of some DL-amino acids and the stability study firmly illustrate the potential of click chemistry for preparation chiral stationary phase for ligand exchange chromatography.

  16. Preparing arbitrary pure states of spatial qudits with a single phase-only spatial light modulator

    CERN Document Server

    Solís-Prosser, M A; Varga, J J M; Rebón, L; Ledesma, S; Iemmi, C; Neves, L

    2013-01-01

    Spatial qudits are D-dimensional ($D\\geq 2$) quantum systems carrying information encoded in the discretized transverse momentum and position of single photons. We present a proof-of-principle demonstration of a method for preparing arbitrary pure states of such systems by using a single phase-only spatial light modulator (SLM). The method relies on the encoding of the complex transmission function corresponding to a given spatial qudit state onto a preset diffraction order of a phase-only grating function addressed at the SLM. Fidelities of preparation above 94% were obtained with this method, which is simpler, less costly, and more efficient than those that require two SLMs for the same purpose.

  17. Improved Procedure for Preparation of Covalently Bonded Cellulose Tris-phenylcarbamate Chiral Stationary Phases

    Institute of Scientific and Technical Information of China (English)

    秦峰; 陈小明; 刘月启; 邹汉法; 王俊德

    2005-01-01

    The classical method for preparation of covalently boned cellulose derivative chiral stationary phases (CSP) with diisocyanate as spacer was improved. Diisocyanate was firstly allowed to react with 3-aminopropyltriethoxysilane, and the resulting product was then applied as the spacer reagent to immobilize cellulose derivatives onto silica gel. Influences of the amount and the length of the spacer on the optical resolution ability of the CSP were investigated. Comparing improved procedure to classical diisocyanate method, the cross-linking between the glucose units of the cellulose derivatives was avoided to the most extent. With the improved procedure, regio-nonselective ways could be adooted to prepare covalently bonded CSP, which showed an advantage for the rapid preparation.

  18. Phase, morphology, and dimension control of CIS powders prepared using a solvothermal process

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Chih-Hui [Department of Materials Science and Engineering, National Cheng Kung University, Tainan, Taiwan (China); Ting, Jyh-Ming, E-mail: jting@mail.ncku.edu.t [Department of Materials Science and Engineering, National Cheng Kung University, Tainan, Taiwan (China)

    2009-05-29

    Crystalline chalcopyrite semiconductor CuInSe{sub 2} nanostructures were prepared using a solvothermal route. Various amine organic agents were used as the solvents. Cupric chloride, indium chloride, and selenium powders were mixed in a solvent of ethylenediamine or diethylamine. Effects of reaction time, reaction temperature, solvent type, and reactant concentration were studied. The results show that through selective processing conditions, the phase, morphology, and dimensions of the obtained CIS nanostructures can be controlled.

  19. Energy Storage Properties of Phase Change Materials Prepared from PEG/CPP

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    New kinds of solid-solid phase change materials have been prepared in our laboratory.In these materials, the rigid polymer chlorinated polypropylene is taken as skeletons and the flexible polymer polyethylene glycol 6000 and polyethylene glycol 10000 are taken as functional chains. Results show that chlorinated polypropylene grafted by polyethylene glycol 10000 has greater enthalpy than chlorinated polypropylene grafted by polyethylene glycol 6000.

  20. PREPARATION OF MICROGEL-EPOXY RESIN TWO-PHASE POLYMERS BY IN SITU POLYMERIZATION

    Institute of Scientific and Technical Information of China (English)

    YU Yunzhao; WU Xianghong; SONG Aiteng

    1991-01-01

    Microgel-epoxy resin two-phase polymers were prepared by in situ copolymerization of ethylenic monomers with unsaturated polyesters. The choice of monomers and the effect of monomer concentration on microgel particle size were discussed. Agglomeration of particles played a significant role in the early stage of polymerization. The microgel dispersion in epoxy resin was stable after the finish of polymerization. Upon curing the particles remained well dispersed.

  1. Mixed phases of TiO2 nanopowders prepared by laser pyrolysis

    Science.gov (United States)

    Dumitrache, Florian V.; Alexandrescu, Rodica; Morjan, Ion G.; Sandu, Ion C.; Soare, Iuliana; Voicu, Ion N.; Fleaca, Claudiu T.; Ploscaru, Mihaela I.; Savoiu, M.; Vasile, Eugen; Ciupina, Victor

    2004-10-01

    TiO2 nano powder was prepared by laser pyrolysis of gas phase reactants. TiCl4 (vapor) was used as titanium precursor. The crystalline structures and morphologies of the powder have been analyzed by transmission electron microscopy (TEM), selected area electron diffraction (SAD) and Raman spectrometry. The different characterization techniques suggest that a nano-crystalline mixture of anatase and rutile is obtained.

  2. PREPARATION OF ZINC OXIDE AND POLY-ETHYLENE OXIDE COMPOSITE MEMBRANES AND THEIR PHASE RELATIONSHIP

    OpenAIRE

    JESÚS FABIAN JURADO; CARLOS VARGAS HERNÁNDEZ; RUBÉN ANTONIO VARGAS

    2012-01-01

    Zinc oxide and organic polymer (poly-ethylene oxide) based nanocomposite membranes were prepared and their phase relationship investigated. The composites were characterized by XRD, Raman scattering, DSC, and impedance spectroscopy analysis. It was found that embedding inorganic nanoparticles of ZnO into the polymer matrix of PEO allowed for some crystallinity formation, and cross-linking of the polymer composites during annealing or synthesis. The XRD and Raman scattering results show more d...

  3. Cell-laden microgel prepared using a biocompatible aqueous two-phase strategy.

    Science.gov (United States)

    Liu, Yang; Nambu, Natalia Oshima; Taya, Masahito

    2017-09-01

    Microfluidic methods are frequently used to produce cell-laden microgels for various biomedical purposes. Such microfluidic methods generally employ oil-water systems. The poor distribution of crosslinking reagents in the oil phase limits the available gelation strategies. Extracting the microgel from the oil-phase also reduces its production efficiency. In this study, an aqueous two-phase system (ATPS) involving dextran (DEX) and polyethylene glycol (PEG) was used to prepare cell-laden microgel. This avoided the problems associated with an oil phase. The microgel precursor polymers and crosslinking reagents were dispersed in the DEX and PEG phases, respectively. The ultra-low interfacial tension of the ATPS hindered droplet formation. A co-flow microfluidic device was fabricated to overcome this problem. The device incorporated a square-wave-changing injection force, to improve the efficiency of droplet formation. The microgel precursor (including alginate and carboxymethyl cellulose derivatives possessing phenolic hydroxyl moieties) could be dispersed in the DEX solution at various concentrations. Uniform droplets were formed with controllable diameters, and were sequentially converted to microgel by horseradish peroxidase-catalyzed crosslinking. Cells were dispersed in the DEX phase with the microgel precursor polymer, and retained their high viability and proliferation in the resulting microgel. The solubility of gelatin derivatives in the DEX phase was low, but was sufficient to impart cell adhesion properties on the microgel.

  4. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    Directory of Open Access Journals (Sweden)

    Helena Prosen

    2014-05-01

    Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  5. Nanosized cobalt-based catalyst prepared by supercritical phase condition for Fischer-Tropsch synthesis

    Institute of Scientific and Technical Information of China (English)

    Jingmiao Li; Jingchang Zhang; Runduo Zhang; Weiliang Cao

    2009-01-01

    A series of nanosized Co/Zn/Mn/K composite catalysts for Fischer-Tropsch synthesis (FTS) were prepared by supercritical fluid drying (SCFD) method and common drying (CD) method. The nanosized cobalt-based catalysts were characterized by XRD,TEM and BET techniques. Their catalytic performances were tested in a slurry-bed reactor under FTS reaction conditions. The drying and crystallization were carded out simultaneously during SCFD,therefore,the catalysts prepared by SCFD method have ideal structure and show the FTS performance superior to the others prepared by CD method. The FTS activity and selectivity were improved via adding Zn,Mn and K promoters,and less CH_4 and CO_2 as well as higher yield of C~(5+) products were achieved. The optimal performance of a 92% CO conversion and a 65% C~(5+) product yield was obtained over a catalyst with the component of Co/Zn/Mn/K = 100/50/10/7. Furthermore,the catalytic performance was studied under the conditions of liquid-phase and supercriticai phase slurry-bed,and C~(5+) product yield were 57.4% and 65.4%,respectively. In summary,better catalytic performance was obtained using the nanosized catalyst prepared by SCFD method under supercritical reaction conditions,resulting in higher conversion of CO,less CO_2 byproduct,and higher yield of C~(5+) products,

  6. Photoluminescence enhancement of YAG:Ce3+ phosphor prepared by co-precipitation-rheological phase method

    Institute of Scientific and Technical Information of China (English)

    YE Xinyu; LONG Zhen; YANG Youming; NIE Huaping; GUO Yanwei; CAI Yufa

    2012-01-01

    YAG:Ce3+ phosphor was prepared by a novel co-precipitation-rheological phase method.The resulting YAG:Ce3+ phosphor was characterized by X-ray diffraction (XRD),scanning electron microscopy (SEM) and photoluminescent emission spectra.By using acetic acid as solvent,YAG:Ce3+ powder with small particle size (≤2 μm) was obtained at a relatively lower sintering temperature of 1400 ℃.With the content of acetic acid increasing,small particles dissolved and disappeared,but larger particles grew up and changed its shape from spherical to partially rectangular.Meanwhile,the emission intensity of the sample prepared by co-precipitation-rheological phase method was about 43% higher than that of the sample prepared by co-precipitation method.It was assumed that the significant improvement of luminescence was mainly because the rheological phase presented a better diffusion environment,and therefore,a better homogeneity of activators of Ce3+.

  7. Decomposition of BN and formation of Nd2Fe14BNx phase prepared by mechanical alloying

    Science.gov (United States)

    Liu, W.; Zhang, Z. D.; Sun, X. K.; He, J. F.; Zhao, X. G.

    1999-07-01

    The decomposition of pyrolytic boron nitride (p-BN) during milling is studied as a function of the milling time. It has been found that the p-BN compound can be partially decomposed by milling until an amorphous p-BN phase is formed so that the content of nitrogen in the p-BN system will not continue to be changed by the milling process. Furthermore, the structure and magnetic properties of Nd2Fe14BNx-based alloys prepared by mechanical alloying using either p-BN or milled p-BN as starting material have been investigated. The Nd2Fe14BNx phase with x up to 0.25 coexists with some amounts of NdN, the Nd-rich phase and icons/Journals/Common/alpha" ALT="alpha" ALIGN="TOP"/>-Fe. A pre-milling process of p-BN favours the formation of the Nd2Fe14BNx phase. The magnetic properties of Nd16Fe76B8Nx alloys prepared by using milled p-BN are better than those made of non-milled p-BN. The Curie temperature of the Nd2Fe14BN0.25 phase is 335 °C, which is slightly higher than that of the Nd2Fe14B compound. A coercivity higher than 20 kOe is achieved for Nd2Fe14BNx-based alloys by adding excess Nd, which is close to the value of Nd16Fe76B8 prepared by using pure B.

  8. Identifying the representative flow unit for capillary dominated two-phase flow in porous media using morphology-based pore-scale modeling

    Science.gov (United States)

    Mu, Yaoming; Sungkorn, Radompon; Toelke, Jonas

    2016-09-01

    In this paper, we extend pore-morphology-based methods proposed by Hazlett (1995) and Hilpert and Miller (2001) to simulate drainage and imbibition in uniformly wetting porous media and add an (optional) entrapment of the (non-)wetting phase. By improving implementation, this method allows us to identify the statistical representative elementary volume and estimate uncertainty by computing fluid flow properties and saturation distributions of hundreds of subsamples within a reasonable time-frame. The method was utilized to study three different porous medium systems and results demonstrate that morphology-based pore-scale modeling is a viable approach to assess the representative elementary volume with respect to capillary dominated two-phase flow. The focus of this paper is the determination of the representative elementary volume for multiphase-flow properties for a digital representation of a rock.

  9. "Chromoseratops Meiosus": A Simple, Two-Phase Exercise to Represent the Connection between Meiosis & Increased Genetic Diversity

    Science.gov (United States)

    Eliyahu, Dorit

    2014-01-01

    I present an activity to help students make the connection between meiosis and genetic variation. The students model meiosis in the first phase of the activity, and by that process they produce gametes of a fictitious reptilobird species, "Chromoseratops meiosus." Later on, they will "mate" their gametes and produce a zygote…

  10. "Chromoseratops Meiosus": A Simple, Two-Phase Exercise to Represent the Connection between Meiosis & Increased Genetic Diversity

    Science.gov (United States)

    Eliyahu, Dorit

    2014-01-01

    I present an activity to help students make the connection between meiosis and genetic variation. The students model meiosis in the first phase of the activity, and by that process they produce gametes of a fictitious reptilobird species, "Chromoseratops meiosus." Later on, they will "mate" their gametes and produce a zygote…

  11. Preparation and Properties of Paraffin/TiO2/Active-carbon Composite Phase Change Materials

    Directory of Open Access Journals (Sweden)

    HAO Yong-gan

    2016-11-01

    Full Text Available A novel composite phase change materials (PCMs of paraffin/TiO2/active-carbon was prepared by a microemulsion method, where paraffin acted as a PCM and titanium dioxide (TiO2 as matrix material, and a small amount of active carbon was added to improve the thermal conductivity. The compositions, morphology and thermal properties of the paraffin/TiO2/active-carbon composite PCMs were characterized by XRD, SEM, TGA and DSC respectively. The shape stability during phase change process of this composite was also tested. The results show that paraffin is well encapsulated by TiO2 matrix, and thus exhibiting excellent shape-stabilized phase change feature. Besides, this composite PCM also presents superhydrophobic property. Therefore, these multifunctional features will endow PCMs with important application potential in energy efficient buildings.

  12. An easily regenerable enzyme reactor prepared from polymerized high internal phase emulsions

    Energy Technology Data Exchange (ETDEWEB)

    Ruan, Guihua, E-mail: guihuaruan@hotmail.com [Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guangxi 541004 (China); Guangxi Collaborative Innovation Center for Water Pollution Control and Water Safety in Karst Area, Guilin University of Technology, Guilin 541004 (China); Wu, Zhenwei; Huang, Yipeng; Wei, Meiping; Su, Rihui [Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guangxi 541004 (China); Du, Fuyou, E-mail: dufu2005@126.com [Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guangxi 541004 (China); Guangxi Collaborative Innovation Center for Water Pollution Control and Water Safety in Karst Area, Guilin University of Technology, Guilin 541004 (China)

    2016-04-22

    A large-scale high-efficient enzyme reactor based on polymerized high internal phase emulsion monolith (polyHIPE) was prepared. First, a porous cross-linked polyHIPE monolith was prepared by in-situ thermal polymerization of a high internal phase emulsion containing styrene, divinylbenzene and polyglutaraldehyde. The enzyme of TPCK-Trypsin was then immobilized on the monolithic polyHIPE. The performance of the resultant enzyme reactor was assessed according to the conversion ability of N{sub α}-benzoyl-L-arginine ethyl ester to N{sub α}-benzoyl-L-arginine, and the protein digestibility of bovine serum albumin (BSA) and cytochrome (Cyt-C). The results showed that the prepared enzyme reactor exhibited high enzyme immobilization efficiency and fast and easy-control protein digestibility. BSA and Cyt-C could be digested in 10 min with sequence coverage of 59% and 78%, respectively. The peptides and residual protein could be easily rinsed out from reactor and the reactor could be regenerated easily with 4 M HCl without any structure destruction. Properties of multiple interconnected chambers with good permeability, fast digestion facility and easily reproducibility indicated that the polyHIPE enzyme reactor was a good selector potentially applied in proteomics and catalysis areas. - Graphical abstract: Schematic illustration of preparation of hypercrosslinking polyHIPE immobilized enzyme reactor for on-column protein digestion. - Highlights: • A reactor was prepared and used for enzyme immobilization and continuous on-column protein digestion. • The new polyHIPE IMER was quite suit for protein digestion with good properties. • On-column digestion revealed that the IMER was easy regenerated by HCl without any structure destruction.

  13. Autonomic-nervous-system activity during the preparation phase for the snatch in Olympic weight lifting.

    Science.gov (United States)

    Collet, Christian; Guillot, Aymeric; Bolliet, Olivier; Dittmar, André

    2006-12-01

    To examine the preparation phase for the snatch lift in Olympic weight lifting. Two behavioral periods were studied, each corresponding to specific mental processes: a stance in front of the bar and placement of hands on the bar. Each period was hypothesized to elicit different responses of autonomic-nervous-system activity. Twelve elite male subjects completed 12 lifts at 90% to 95% of their best grade after warm-up (80% of their best grade). Because peripheral autonomic-nervous-system activity is related to arousal and activation variation, 6 variables were continuously recorded: electrodermal (skin resistance and potential), thermovascular (skin temperature and skin blood flow), and cardiorespiratory (heart rate and respiratory frequency). Responses (ie, phasic activities) were evident during the first behavioral period. Decrease in heart rate (mean = 19 beats/min) or in respiratory frequency (mean = 8.6 beats/min) was related to attention processes. These responses were weaker (-0.16 degrees C vs -0.25 degrees C in skin temperature) and shorter (2.7 seconds vs 4.3 seconds in skin resistance) than those recorded during execution. The second phase showed variations in basal levels (mean increase in heart rate of 25%), related to increase in activation, thus attesting the muscle system's process of preparation for effort. Weight lifters separated the preparation phase into 2 stages that were closely matched by different physiological activities. Weight lifting requires participants to share their mental resources among the 2 demanding concentration phases by first focusing their attention on the execution and then mobilizing energizing resources.

  14. Nanocellulose 3, 5-Dimethylphenylcarbamate Derivative Coated Chiral Stationary Phase: Preparation and Enantioseparation Performance.

    Science.gov (United States)

    Zhang, Xiaoli; Wang, Litao; Dong, Shuqing; Zhang, Xia; Wu, Qi; Zhao, Liang; Shi, Yanping

    2016-05-01

    Nanocrystalline cellulose (NCC) with high surface area and high ordered crystalline structure was prepared from microcrystalline cellulose (MCC) under the hydrolysis of sodium hypochlorite. NCC was further reacted with 3,5-dimethylphenyl isocyanate to obtain the nanocellulose derivative, and then coated successfully on the surface of silica gel to a prepared NCC-coated chiral stationary phase (CSP) as a new kind of chiral separation material. Similarly, MCC derivative-coated CSP was also prepared as contrast. The chiral separation performance of NCC-based CSP was evaluated and compared with MCC-based CSP by high-performance liquid chromatography. Moreover, the effects of the alcohol modifiers, mobile phase additives, and flow rates on chiral separations were investigated in detail. The results showed that 10 chiral compounds were separated on NCC-based CSP with better peak shape and higher column efficiency than MCC-based CSP, which confirmed that NCC-based CSP was a promising packing material for the resolution of chiral compounds.Chirality 28:376-381, 2016. © 2016 Wiley Periodicals, Inc.

  15. An easily regenerable enzyme reactor prepared from polymerized high internal phase emulsions.

    Science.gov (United States)

    Ruan, Guihua; Wu, Zhenwei; Huang, Yipeng; Wei, Meiping; Su, Rihui; Du, Fuyou

    2016-04-22

    A large-scale high-efficient enzyme reactor based on polymerized high internal phase emulsion monolith (polyHIPE) was prepared. First, a porous cross-linked polyHIPE monolith was prepared by in-situ thermal polymerization of a high internal phase emulsion containing styrene, divinylbenzene and polyglutaraldehyde. The enzyme of TPCK-Trypsin was then immobilized on the monolithic polyHIPE. The performance of the resultant enzyme reactor was assessed according to the conversion ability of Nα-benzoyl-l-arginine ethyl ester to Nα-benzoyl-l-arginine, and the protein digestibility of bovine serum albumin (BSA) and cytochrome (Cyt-C). The results showed that the prepared enzyme reactor exhibited high enzyme immobilization efficiency and fast and easy-control protein digestibility. BSA and Cyt-C could be digested in 10 min with sequence coverage of 59% and 78%, respectively. The peptides and residual protein could be easily rinsed out from reactor and the reactor could be regenerated easily with 4 M HCl without any structure destruction. Properties of multiple interconnected chambers with good permeability, fast digestion facility and easily reproducibility indicated that the polyHIPE enzyme reactor was a good selector potentially applied in proteomics and catalysis areas.

  16. Preparation of fluorescent DNA probe by solid-phase organic synthesis

    Directory of Open Access Journals (Sweden)

    2009-08-01

    Full Text Available Fluorescent DNA probe based on fluorescence resonance energy transfer (FRET was prepared by solid-phase organic synthesis when CdTe quantum dots (QDs were as energy donors and Au nanoparticles (AuNPs were as energy accepters. The poly(divinylbenzene core/poly(4-vinylpyridine shell microspheres, as solid-phase carriers, were prepared by seeds distillation-precipitation polymerization with 2,2′-azobisisobutyronitrile (AIBN as initiator in neat acetonitrile. The CdTe QDs and AuNPs were self-assembled on the surface of core/shell microspheres, and then the linkage of CdTe QDs with oligonucleotides (CdTe-DNA and AuNPs with complementary single-stranded DNA (Au-DNA was on the solid-phase carriers instead of in aqueous solution. The hybridization of complementary double stranded DNA (dsDNA bonded to the QDs and AuNPs (CdTe-dsDNA-Au determined the FRET distance of CdTe QDs and AuNPs. Compared with the fluorescence of CdTe-DNA, the fluorescence of CdTe-dsDNA-Au conjugates (DNA probes decreased extremely, which indicated that the FRET occurred between CdTe QDs and AuNPs. The probe system would have a certain degree recovery of fluorescence when the complementary single stranded DNA was introduced into this system, which showed that the distance between CdTe QDs and AuNPs was increased.

  17. UV irradiation-initiated MMA polymerization to prepare microcapsules containing phase change paraffin

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Sude; Song, Guolin; Li, Wei; Fan, Pengfei; Tang, Guoyi [Institute of Advanced Materials, Graduated School at Shenzhen, Tsinghua University, Shenzhen 518055 (China)

    2010-10-15

    Microencapsulated phase change material (MEPCM), paraffin, with polymethylmethacrylate shell was prepared by introducing UV irradiation to an O/W emulsion polymerization for approximately 30 min under constant stirring. The results of differential scanning calorimetry analyses indicate that the latent heat and the content of paraffin of microcapsules are 101 J g{sup -1} and 61.2 wt%, respectively. The phase transition temperature of MEPCM ranges from 24 to 33 C. The MEPCM was characterized using scanning electron microscopy and Fourier transform infrared spectroscopy. Thermal gravimetric analysis results show that the MEPCM is degraded into two distinguishable steps. Accelerated thermal cycling tests also indicate that the MEPCM displays a good thermal reliability. Gypsum boards composed of as-prepared MEPCM show a good temperature-regulated property. Based on all these results, it can be concluded that the microencapsulated paraffin as MEPCMs have good potential for thermal energy storage purposes such as phase change material slurries, solar space heating applications, textiles and building materials. (author)

  18. PHASE STRUCTURE AND COMPATIBILITY OF LADDERLIKE POLYPHENYLSILSESQUIOXANE (PPSQ)/POLYCARBONATE (PC) BLENDS PREPARED BY SOLUTION CASTING

    Institute of Scientific and Technical Information of China (English)

    Gui-zhi Li; Liang-he Shi

    1999-01-01

    Blends of PC and PPSQ (A) with high Mw and good ladderlike regularity or PPSQ(B) with low Mw and more defective Si-atoms in its structure have been prepared by solution casting. The dispersed spheres (PPSQ(A)-rich) are unevenly dispersed in the continuous PC-rich phase and there is no phase-inversion as PPSQ(A) content increases when the percentage of PPSQ(A) is not more than70%. PPSQ(B)-rich spheres are evenly dispersed in the continuous phase (PC-rich) and phaseinversion occurs when PPSQ(B) percentage is up to 70%. Tg of PPSQ(A)/PC or PPSQ(B)/PC at some compositions are lower than that of pure PC due to the enlarged free-volume of PC-rich phase because some spheres of rigid PPSQ chains are included in the PC-rich phase. PC and PPSQ(A) or PPSQ(B)are partially compatible. The compatibility of PC and PPSQ(B) is better than that of PC and PPSQ(A)with high Mw and good ladderlike regularity. Heat history has some influence on the TgS and compatibility of PPSQ(A)/PC and PPSQ(B)/PC blends.

  19. Preparation and Characterization of a New Quercetin-bonded Stationary Phase for High Performance Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    李来生; 方奕珊; 陈红; 张杨

    2012-01-01

    A quercetin-bonded silica gel stationary phase (QUSP) containing natural flavonoid ligand was first prepared via γ-glycidoxypropyltrimethoxysilane (KH-560) as a coupling reagent for high-performance liquid chromatography. Its chemical structure was characterized by Fourier infrared spectroscopy, elemental analysis, thermal thermogravimetry and 13C cross polarization/magic angle spinning nuclear magnetic resonance (CP/MAS NMR). The chromatographic property of QUSP was systematically evaluated by using neutral, basic and acidic aromatic com- pounds as probes. In order to clarify its retention mechanism, a comparative study of QUSP with conventional oc- tadecylsilyl-bonded stationary phase (ODS) was also carried out under the same conditions. The results showed that the new quercetin-bonded phase exhibited an excellent reversed-phase chromatographic property with relatively weak hydrophobicity. However, it has an advantage over ODS in the fast separation of polar aromatic compounds because the quercetin ligand could provide various sites besides hydrophobicity, such as hydrogen bonding, dipole-dipole, n-n staking and charge transfer interactions. QUSP was performed in the baseline separations of ion- ized polar basic or acidic compounds, including pyridines, anilines, pyrimidines, purines and phenols with symmet- ric peak shape in common mobile phases without buffer salt within relatively short time. The natural ligands from herbs are readily available and contain a variety of active sites, which facilitate the exploration of industrial chromatographic separation materials for green products.

  20. Purification of flavonoids from licorice using an off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method.

    Science.gov (United States)

    Fan, Yunpeng; Fu, Yanhui; Fu, Qing; Cai, Jianfeng; Xin, Huaxia; Dai, Mei; Jin, Yu

    2016-07-01

    An orthogonal (71.9%) off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method coupled with effective sample pretreatment was developed for separation and purification of flavonoids from licorice. Most of the nonflavonoids were firstly removed using a self-made Click TE-Cys (60 μm) solid-phase extraction. In the first dimension, an industrial grade preparative chromatography was employed to purify the crude flavonoids. Click TE-Cys (10 μm) was selected as the stationary phase that provided an excellent separation with high reproducibility. Ethyl acetate/ethanol was selected as the mobile phase owing to their excellent solubility for flavonoids. Flavonoids co-eluted in the first dimension were selected for further purification using reversed-phase liquid chromatography. Multiple compounds could be isolated from one normal-phase fraction and some compounds with bad resolution in one-dimensional liquid chromatography could be prepared in this two-dimensional system owing to the orthogonal separation. Moreover, this two-dimensional liquid chromatography method was beneficial for the preparation of relatively trace flavonoid compounds, which were enriched in the first dimension and further purified in the second dimension. Totally, 24 flavonoid compounds with high purity were obtained. The results demonstrated that the off-line two-dimensional liquid chromatography method was effective for the preparative separation and purification of flavonoids from licorice.

  1. Preparation and initial characterization of fluidized bed steam reforming pure-phase standards

    Energy Technology Data Exchange (ETDEWEB)

    Missimer, D. M.; Rutherford, R. L.

    2013-03-21

    Hanford is investigating the Fluidized Bed Steam Reforming (FBSR) process for their Low Activity Waste. The FBSR process offers a low-temperature continuous method by which liquid waste can be processed with the addition of clay into a sodium aluminosilicate (NAS) waste form. The NAS waste form is mainly comprised of nepheline (NaAlSiO{sub 4}), sodalite (Na{sub 8}[AlSiO{sub 4}]{sub 6}Cl{sub 2}), and nosean (Na{sub 8}[AlSiO{sub 4}]{sub 6}SO{sub 4}). Anions such as perrhenate (ReO{sub 4}{sup -}), pertechnetate (TcO{sub 4}{sup -}), and iodine (I{sup -}) are expected to replace sulfate in the nosean structure and/or chloride in the sodalite mineral structure (atomically bonded inside the aluminosilicate cages that these mineral structures possess). In the FBSR waste form, each of these phases can exist in a variety of solid solutions that differ from the idealized forms observed in single crystals in nature. The lack of understanding of the durability of these stoichiometric or idealized mineral phases complicates the ability to deconvolute the durability of the mixed phase FBSR product since it is a combination of different NAS phases. To better understand the behavior, fabrication and testing of the individual phases of the FBSR product is required. Analytical Development (AD) of the Science and Technology directorate of the Savannah River National Laboratory (SRNL) was requested to prepare the series of phase-pure standards, consisting of nepheline, nosean, and Cl, Re, and I sodalite. Once prepared, X-ray Diffraction (XRD) analyses were used to confirm the products were phase pure. These standards are being used for subsequent characterization studies consisting of the following: single-pass flow-through (SPFT) testing, development of thermodynamic data, and x-ray diffraction (XRD) calibration curves. In addition to the above mentioned phase-pure standards, AD was tasked with fabricating a mixed Tc-Re sodalite.

  2. Characterization of Polysulfone Membranes Prepared with Thermally Induced Phase Separation Technique

    Science.gov (United States)

    Tiron, L. G.; Pintilie, Ș C.; Vlad, M.; Birsan, I. G.; Baltă, Ș

    2017-06-01

    Abstract Membrane technology is one of the most used water treatment technology because of its high removal efficiency and cost effectiveness. Preparation techniques for polymer membranes show an important aspect of membrane properties. Generally, polysulfone (PSf) and polyethersulfone (PES) are used for the preparation of ultrafiltration (UF) membranes. Polysulfone (PSf) membranes have been widely used for separation and purification of different solutions because of their excellent chemical and thermal stability. Polymeric membranes were obtained by phase inversion method. The polymer solution introduced in the nonsolvent bath (distilled water) initiate the evaporation of the solvent from the solution, this phenomenon has a strong influence on the transport properties. The effect of the coagulation bath temperature on the membrane properties is of interest for this study. Membranes are characterized by pure water flux, permeability, porosity and retention of methylene blue. The low temperature of coagulation bath improve the membrane’s rejection and its influence was most notable.

  3. Preparation and photoelectric property of TiO{sub 2} nanoparticles with controllable phase junctions

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Hongmei [School of Environmental Science and Engineering, Tianjin University, Tianjin 300072 (China); Tan, Xin [School of Science, Tibet University, Lhasa 850000, Tibet (China); Yu, Tao, E-mail: yutao@tju.edu.cn [School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Tianjin University-National Institute for Materials Science (TU-NIMS) Joint Research Center, Tianjin University, Tianjin 300072 (China)

    2014-12-01

    Graphical abstract: - Highlights: • A series of bicrystalline TiO{sub 2} nanoparticles with different ratio of controllable phase junctions between anatase and rutile were synthesized successfully using ionic liquid-assisted method by hydrolysis of TiCl{sub 4}. • The spatial separation capacity of photogenerated charge carriers and photocatalytic activities of the samples with different ratio of controllable phase junctions were evaluated systemically. • The best photocatalytic activity for MO degradation can reach above 99% at the sample with 27.4% rutile which also has the best photoelectric property compared with other samples. - Abstract: To explore the effect of phase composition on the photoelectric property of anatase–rutile mixed crystal nanoparticles, a series of TiO{sub 2} nanoparticles with phase junctions controlling were synthetized by hydrolysis of TiCl{sub 4} in hydrochloric acid, an ionic liquid-assisted method was used during this process. Crystalline size and the ratio of anatase to rutile of as-prepared samples were calculated by the XRD. The surface area was measured by nitrogen sorption measurements using the BET method. The micro-structure of phase junctions was characterized by TEM. Optical transmittance properties of TiO{sub 2} with controllable phase junctions were examined via ultraviolet–visible diffuse reflection spectroscopy (UV–vis DRS). The particles were manufactured into films using the doctor-blade technique on FTO glasses. To test photocurrent density, and spatial separation capacity of electron–holes pairs, photo-electro method was employed. The photocatalytic activities of the resulting samples were examined in the degradation of methyl orange (MO) under artificial solar light irradiation. Mechanisms of separation and transfer of photogenerated charge and the effect of phase composition on photoelectric property of anatase–rutile nanoparticles were discussed.

  4. Preparation of A New Fiber by Sol-gel Technology in Solid-phase Microextraction (SPME)

    Institute of Scientific and Technical Information of China (English)

    Li Ming WEI; Qing Yu OU; Ju Bai LI

    2004-01-01

    The sol-gel technology is applied for the preparation of solid-phase microextraction (SPME) fiber. The fiber demonstrates high thermal stability, efficient extraction rate and the selectivity for non-polar or low-polar analytes. Efficient SPME-GC-FID analyses of benzene- toluene-ethylbenzene-xylenes (BTEXs) and low-polar halocarbon were achieved by the sol-gel coated DSDA-DDBT-TiO2 fiber. Some parameters of the SPME fiber for the determination of halocarbon in aqueous sample were investigated.

  5. Implementation of quantum controlled phase gate and preparation of multiparticle entanglement in cavity QED

    Institute of Scientific and Technical Information of China (English)

    Wu Xi; Chen Zhi-Hua; Zhang Yong; Chen Yue-Hua; Ye Ming-Yong; Lin Xiu-Min

    2011-01-01

    Schemes are presented for realizing quantum controlled phase gate and preparing an N-qubit W-like state, which are based on the large-detuned interaction among three-state atoms, dual-mode cavity and a classical pulse. In particular, a class of W states that can be used for perfect teleportation and superdense coding is generated by only one step.Compared with the previous schemes, cavity decay is largely suppressed because the cavity is only virtually excited and always in the vacuum state and the atomic spontaneous emission is strongly restrained due to a large atom-field detuning.

  6. Exploring solid-phase approaches for the preparation of new beta-lactams from amino acids.

    Science.gov (United States)

    Gerona-Navarro, Guillermo; Royo, Miriam; García-López, Ma Teresa; Albericio, Fernando; González-Muñiz, Rosario

    2003-01-01

    Two solid-phase approaches, involving the base-assisted intramolecular alkylation of N-chloroacetyl-Phe derivatives anchored to appropriate solid supports, were investigated for the preparation of novel beta-lactams. When a BAL-type strategy was used, the resin-bound azetidinones were easily formed, as established by MAS-NMR, but final compounds could not be removed from the resin, unless a suitable two linkers system was used. In the second approach, in which the Phe residue is anchored to a Wang-type resin through the carboxylate group, the corresponding 1,4,4-trisubstituted 2-azetidinone was obtained in moderate to good yield and high purity.

  7. Effect of Heat Treatment on Mechanical Properties and Phase Composition of Magnesium-Aluminum Composite Prepared by Explosive Welding

    Science.gov (United States)

    Arisova, V. N.; Trykov, Yu. P.; Slautin, O. V.; Ponomareva, I. A.; Kondakov, A. E.

    2015-09-01

    Results are given for a study of the effect of heat treatment regimes on the nature of change in micromechanical properties and phase composition of magnesium-aluminum composite material AD1-MA2-1 prepared by explosive welding.

  8. Preparation of bioconjugates by solid-phase conjugation to ion exchange matrix-adsorbed carrier proteins

    DEFF Research Database (Denmark)

    Houen, G.; Olsen, D.T.; Hansen, P.R.;

    2003-01-01

    A solid-phase conjugation method utilizing carrier protein bound to an ion exchange matrix was developed. Ovalbumin was adsorbed to an anion exchange matrix using a batch procedure, and the immobilized protein was then derivatized with iodoacetic acid N-hydroxysuccinimid ester. The activated......, and immunization experiments with the eluted conjugates showed that the more substituted conjugates gave rise to the highest titers of glutathione antibodies. Direct immunization with the conjugates adsorbed to the ion exchange matrix was possible and gave rise to high titers of glutathione antibodies. Conjugates...... of ovalbumin and various peptides were prepared in a similar manner and used for production of peptide antisera by direct immunization with the conjugates bound to the ion exchanger. Advantages of the method are its solid-phase nature, allowing fast and efficient reactions and intermediate washings...

  9. Pt nanoparticles on titania nanotubes prepared by vapor-phase impregnation-decomposition method

    Energy Technology Data Exchange (ETDEWEB)

    Encarnacion Gomez, C. [National Polytechnic Institute, Dept. of Metallurgical Eng., Mexico 07300 DF, AP 75-874 (Mexico); Vargas Garcia, J.R., E-mail: rvargasga@ipn.m [National Polytechnic Institute, Dept. of Metallurgical Eng., Mexico 07300 DF, AP 75-874 (Mexico); Toledo Antonio, J.A.; Cortes Jacome, M.A.; Angeles Chavez, C. [Petroleum Mexican Institute, Eje Central Lazaro Cardenas No. 152, Mexico 07730 DF (Mexico)

    2010-04-16

    Platinum (Pt) nanoparticles were prepared on titania nanotubes (TNTs) by vapor-phase impregnation-decomposition method using platinum acetylacetonate as precursor. TNTs and Pt precursor were mixed in 3:1 weight ratio before vapor-phase impregnation. The mixed powders were heated at 453 K for 10 min to evaporate the precursor in a horizontal tube quartz reactor at a total pressure of 66.6 kPa. Then, the impregnated TNTs were moved to a higher temperature zone (673 K) inside the tube reactor to achieve the precursor decomposition. HAADF-STEM observations, AAS and XPS results revealed that this method allows the formation of uniformly distributed Pt nanoparticles on the surface of TNTs with a narrow distribution of particle size (2.1 nm mean size). Pt nanoparticles remain mainly as Pt{sup 0} oxidation state with a Pt{sup 0}/Pt{sup 2+} atomic ratio of 3.9.

  10. Streamlined Membrane Proteome Preparation for Shotgun Proteomics Analysis with Triton X-100 Cloud Point Extraction and Nanodiamond Solid Phase Extraction

    OpenAIRE

    Pham, Minh D.; Ting-Chun Wen; Hung-Cheng Li; Pei-Hsuan Hsieh; Yet-Ran Chen; Huan-Cheng Chang; Chau-Chung Han

    2016-01-01

    While mass spectrometry (MS) plays a key role in proteomics research, characterization of membrane proteins (MP) by MS has been a challenging task because of the presence of a host of interfering chemicals in the hydrophobic protein extraction process, and the low protease digestion efficiency. We report a sample preparation protocol, two-phase separation with Triton X-100, induced by NaCl, with coomassie blue added for visualizing the detergent-rich phase, which streamlines MP preparation fo...

  11. Preparation of CMC-modified melamine resin spherical nano-phase change energy storage materials.

    Science.gov (United States)

    Hu, Xiaofeng; Huang, Zhanhua; Zhang, Yanhua

    2014-01-30

    A novel carboxymethyl cellulose (CMC)-modified melamine-formaldehyde (MF) phase change capsule with excellent encapsulation was prepared by in situ polymerization. Effects of CMC on the properties of the capsules were studied by Fourier transformation infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), scanning electronic microscopy (SEM), X-ray diffractometry (XRD), and thermogravimetric analysis (TGA). The results showed that the CMC-modified capsules had an average diameter of about 50nm and good uniformity. The phase change enthalpy of the capsules was increased and the cracking ratio decreased by incorporating a suitable amount of CMC. The optimum phase change enthalpy of the nanocapsules was 83.46J/g, and their paraffin content was 63.1%. The heat resistance of the capsule shells decreased after CMC modification. In addition, the nanocapsule cracking ratio of the nanocapsules was 11.0%, which is highly attractive for their application as nano phase change materials. Copyright © 2013 Elsevier Ltd. All rights reserved.

  12. Preparation

    Directory of Open Access Journals (Sweden)

    M.M. Dardir

    2014-03-01

    Full Text Available Some hexanamide-mono and di-linoleniate esters were prepared by the reaction of linolenic acid and hexanamide (derived from the reaction of hexanoic acid and diethanolamine. The chemical structure for the newly prepared hexanamide-mono and di-linoleniate esters were elucidated using elemental analysis, (FTIR, H 1NMR and chemical ionization mass spectra (CI/Ms spectroscopic techniques. The results of the spectroscopic analysis indicated that they were prepared through the right method and they have high purity. The new prepared esters have high biodegradability and lower toxicity (environmentally friendly so they were evaluated as a synthetic-based mud (ester-based mud for oil-well drilling fluids. The evaluation included study of the rheological properties, filtration and thermal properties of the ester based-muds formulated with the newly prepared esters compared to the reference commercial synthetic-based mud.

  13. Nb 28Ni 33.5Sb 12.5, a New Representative of the X-phase

    Science.gov (United States)

    Wang, Meitian; Mar, Arthur

    2001-09-01

    The first ternary compound in the Nb-Ni-Sb system, Nb28Ni33.5Sb12.5, has been synthesized and its structure has been determined by single-crystal X-ray diffraction methods. Nb28Ni33.5(2)Sb12.5(2) adopts the X-phase structure type (orthorhombic, space group Pnnm, Z=1, a=13.2334(5) Å, b=16.5065(7) Å, c=5.0337(2) Å), which belongs to the set of tetrahedrally close-packed (TCP) structures adopted by many intermetallic compounds. Typical of such TCP structures, the atoms reside in sites of high coordination number, with Ni and Sb in CN12 and Nb in CN14, -15, and -16 sites. The relative importance of various metal-metal bonding interactions is discussed on the basis of extended Hückel band structure calculations. Nb28Ni33.5Sb12.5 displays metallic behavior with a room-temperature resistivity of 2.3×10-4 Ω cm.

  14. Matrix compatible solid phase microextraction coating, a greener approach to sample preparation in vegetable matrices.

    Science.gov (United States)

    Naccarato, Attilio; Pawliszyn, Janusz

    2016-09-01

    This work proposes the novel PDMS/DVB/PDMS fiber as a greener strategy for analysis by direct immersion solid phase microextraction (SPME) in vegetables. SPME is an established sample preparation approach that has not yet been adequately explored for food analysis in direct immersion mode due to the limitations of the available commercial coatings. The robustness and endurance of this new coating were investigated by direct immersion extractions in raw blended vegetables without any further sample preparation steps. The PDMS/DVB/PDMS coating exhibited superior features related to the capability of the external PDMS layer to protect the commercial coating, and showed improvements in terms of extraction capability and in the cleanability of the coating surface. In addition to having contributed to the recognition of the superior features of this new fiber concept before commercialization, the outcomes of this work serve to confirm advancements in the matrix compatibility of the PDMS-modified fiber, and open new prospects for the development of greener high-throughput analytical methods in food analysis using solid phase microextraction in the near future.

  15. An Approach to Preparing Ni-P with Different Phases for Use as Supercapacitor Electrode Materials.

    Science.gov (United States)

    Wang, Dan; Kong, Ling-Bin; Liu, Mao-Cheng; Luo, Yong-Chun; Kang, Long

    2015-12-01

    Herein, we describe a simple two-step approach to prepare nickel phosphide with different phases, such as Ni2 P and Ni5 P4 , to explain the influence of material microstructure and electrical conductivity on electrochemical performance. In this approach, we first prepared a Ni-P precursor through a ball milling process, then controlled the synthesis of either Ni2 P or Ni5 P4 by the annealing method. The as-prepared Ni2 P and Ni5 P4 are investigated as supercapacitor electrode materials for potential energy storage applications. The Ni2 P exhibits a high specific capacitance of 843.25 F g(-1) , whereas the specific capacitance of Ni5 P4 is 801.5 F g(-1) . Ni2 P possesses better cycle stability and rate capability than Ni5 P4 . In addition, the Fe2 O3 //Ni2 P supercapacitor displays a high energy density of 35.5 Wh kg(-1) at a power density of 400 W kg(-1) and long cycle stability with a specific capacitance retention rate of 96 % after 1000 cycles, whereas the Fe2 O3 //Ni5 P4 supercapacitor exhibits a high energy density of 29.8 Wh kg(-1) at a power density of 400 W kg(-1) and a specific capacitance retention rate of 86 % after 1000 cycles.

  16. Preparation of graphene/TiO{sub 2} composites by nonionic surfactant strategy and their simulated sunlight and visible light photocatalytic activity towards representative aqueous POPs degradation

    Energy Technology Data Exchange (ETDEWEB)

    Li, Kexin; Xiong, Jingjing; Chen, Tong [Provincial Key Laboratory of Ecological Diagnosis-Remediation and Pollution Blocking Technology, Department of Environment and Chemical Engineering, Nanchang Hangkong Uuniversity, Nanchang 330063 (China); Yan, Liushui, E-mail: yanliushui1964@yahoo.cn [Provincial Key Laboratory of Ecological Diagnosis-Remediation and Pollution Blocking Technology, Department of Environment and Chemical Engineering, Nanchang Hangkong Uuniversity, Nanchang 330063 (China); Dai, Yuhua; Song, Dongyang; Lv, Ying; Zeng, Zhenxing [Provincial Key Laboratory of Ecological Diagnosis-Remediation and Pollution Blocking Technology, Department of Environment and Chemical Engineering, Nanchang Hangkong Uuniversity, Nanchang 330063 (China)

    2013-04-15

    Highlights: ► A series of graphene/TiO{sub 2} composites were developed by nonionic surfactant strategy. ► The textural property, optical property, and composition were well characterized. ► Aqueous POPs were degraded under simulated sunlight and visible light irradiation. ► The degradation mechanism and kinetics of aqueous POPs were studied in detail. ► Mineralization of aqueous POPs and recyclability of the composites were also tested. -- Abstract: A series of graphene/TiO{sub 2} composites were fabricated using a single-step nonionic surfactant strategy combined with the solvothermal treatment technique. Their phase structure, morphology, porosity, optical absorption property, as well as composition and structure, were characterized. The as-prepared composites were successfully applied to degrade aqueous persistent organic pollutants (POPs) such as rhodamine B, aldicarb, and norfloxacin in simulated sunlight (λ > 320 nm) and visible light (λ > 400 nm) irradiation. The degradation mechanism and kinetics of aqueous POPs were studied in detail. The mineralization of aqueous POPs and the recyclability of the composites were also tested in the same condition.

  17. Preparation of Biofuel from Palm Oil Catalyzed by Ammonium Molybdate in Homogeneous Phase

    Directory of Open Access Journals (Sweden)

    Sepehr Sadighi

    2017-04-01

    Full Text Available Producing transportation fuels from bio sources was of prime importance due to the strict environmental legislations for producing clean fuels from conventional oil resources. However, the economical impacts of the biofuel production should be considered. In this study, the production of bio-naphtha and biodiesel from palm oil using homogeneous catalyst, i.e. an aqueous phase of ammonium molybdate, was studied. This catalyst was prepared by dissolving sodium molybdate in de-ionized water with hydrochloric acid, and then neutralizing the mixture with ammonium hydroxide. The solution was dried at 90 °C for 24 h to obtain ammonium molybdate. Then, characterization of the catalyst was done by informative techniques, such as XRD and FT-IR. The results showed that the main phase of the synthesized catalyst was molybdate ammonium hydrates (4MoO3.2NH3.H2O, and also bands of Mo–O, Mo–O–Mo, N–H and surface hydroxyl groups were observed in the sample. Moreover, activity test confirms that the bio-naphtha produced from the proposed method has a few aromatic components, and its sulfur content was negligible. Moreover, ash, nitrogen, sulfur and carbon residue were not detected in the produced biodiesel, and its Cetane index was 66.3. Therefore, it was a suitable fuel for diesel engines vehicles. Copyright © 2017 BCREC GROUP. All rights reserved Received: 3rd May 2016; Revised: 1st October 2016; Accepted: 18th October 2016 How to Cite: Sadighi, S., Targhi, S.K.M. (2017. Preparation of Biofuel from Palm Oil Catalyzed by Ammonium Molybdate in Homogeneous Phase. Bulletin of Chemical Reaction Engineering & Catalysis, 12 (1: 49-54 (doi:10.9767/bcrec.12.1.486.49-54 Permalink/DOI: http://dx.doi.org/10.9767/bcrec.12.1.486.49-54

  18. Strain effects in Nb3Al multifilamentary conductors prepared by phase transformation from bcc supersaturated-solid solution

    NARCIS (Netherlands)

    Takeuchi, T.; Iijima, Y.; Inoue, K.; Wada, H.; Haken, ten B.; Kate, ten H.H.J.; Fukuda, K.; Iwaki, G.; Sakai, S.; Moriai, H.

    1997-01-01

    Strain effects on critical current densities have been examined for conductors containing nearly stoichiometric Nb3Al filaments with fine grains. The Nb3Al phase in these multifilamentary conductors are prepared by phase transformation from supersaturated Nb(Al) bcc solid solution and show high-fiel

  19. Nanocellulose Derivative/Silica Hybrid Core-Shell Chiral Stationary Phase: Preparation and Enantioseparation Performance

    Directory of Open Access Journals (Sweden)

    Xiaoli Zhang

    2016-05-01

    Full Text Available Core-shell silica microspheres with a nanocellulose derivative in the hybrid shell were successfully prepared as a chiral stationary phase by a layer-by-layer self-assembly method. The hybrid shell assembled on the silica core was formed using a surfactant as template by the copolymerization reaction of tetraethyl orthosilicate and the nanocellulose derivative bearing triethoxysilyl and 3,5-dimethylphenyl groups. The resulting nanocellulose hybrid core-shell chiral packing materials (CPMs were characterized and packed into columns, and their enantioseparation performance was evaluated by high performance liquid chromatography. The results showed that CPMs exhibited uniform surface morphology and core-shell structures. Various types of chiral compounds were efficiently separated under normal and reversed phase mode. Moreover, chloroform and tetrahydrofuran as mobile phase additives could obviously improve the resolution during the chiral separation processes. CPMs still have good chiral separation property when eluted with solvent systems with a high content of tetrahydrofuran and chloroform, which proved the high solvent resistance of this new material.

  20. Preparation of meta-stable phases of barium titanate by Sol-hydrothermal method

    Directory of Open Access Journals (Sweden)

    Mahalakshmi Selvaraj

    2015-11-01

    Full Text Available Two low-cost chemical methods of sol–gel and the hydrothermal process have been strategically combined to fabricate barium titanate (BaTiO3 nanopowders. This method was tested for various synthesis temperatures (100 °C to 250 °C employing barium dichloride (BaCl2 and titanium tetrachloride (TiCl4 as precursors and sodium hydroxide (NaOH as mineralizer for synthesis of BaTiO3 nanopowders. The as-prepared BaTiO3 powders were investigated for structural characteristics using x-ray diffraction (XRD, scanning electron microscopy (SEM and transmission electron microscopy (TEM. The overall analysis indicates that the hydrothermal conditions create a gentle environment to promote the formation of crystalline phase directly from amorphous phase at the very low processing temperatures investigated. XRD analysis showed phase transitions from cubic - tetragonal - orthorhombic - rhombohedral with increasing synthesis temperature and calculated grain sizes were 34 – 38 nm (using the Scherrer formula. SEM and TEM analysis verified that the BaTiO3 nanopowders synthesized by this method were spherical in shape and about 114 - 170 nm in size. The particle distribution in both SEM and TEM shows that as the reaction temperature increases from 100 °C to 250 °C, the particles agglomerate. Selective area electron diffraction (SAED shows that the particles are crystalline in nature. The study shows that choosing suitable precursor and optimizing pressure and temperature; different meta-stable (ferroelectric phases of undoped BaTiO3 nanopowders can be stabilized by the sol-hydrothermal method.

  1. Preparation by a Rheological Phase Reaction Method and Thermal Decomposition Reaction Mechanism of Nickelous Salicylate Tetrahydrate

    Institute of Scientific and Technical Information of China (English)

    Wang Jin-long; Yuan Liang-jie; Yang Yi-yong; Sun Ju-tang; Zhang Ke-li

    2003-01-01

    The single crystal nickel salicylate tetrahydrate was prepared with the rheological phase reaction method from nickelous hydroxide and salicylic acid. The crystal structure was determined. It is monoclinic, space group P21 /n, a =0.67874(3), b=0. 515 91(2), c=2. 313 30(9) nm, β=90.9286(17)°, V=0. 809 94(6) nm3, Z=2, ρcalcd =0. 065 0[I >2a(I)]. The thermal decomposition mechanism in an inert atmosphere was investigated via TG, DTG and DTA. The thermal decomposition products were characterized with IR and micro-powder X-ray diffraction method. A new coordination polymer (NiC6 H4O)n as an intermediate product and nanoscale metal nickel were obtained in the ranges of 364-429 ℃ and 429-680 ℃, respectively.

  2. Preparation of graphene sponge by vapor phase reduction for oil and organic solvent removal

    Science.gov (United States)

    Wu, Ruihan; Yu, Baowei; Jin, Xinyan; Liu, Xiaoyang; Bai, Yitong; Chen, Lingyun; Ming, Zhu; Yang, Hua; Yang, Sheng-Tao; Luo, Jianbin

    2016-10-01

    Due to the porous structure and hydrophobicity, graphene sponge has huge adsorption capacity for oils and organic solvents. In this study, we reported that graphene sponge could be prepared by vapor phase reduction (denoted as VPRGS) for oil and organic solvent removal. Graphene oxide was lyophilized and reduced by steamy hydrazine hydrate to produce VPRGS. VPRGS had huge capacity for oils and organic solvents (72–224 g g‑1). In particular, the adsorption capacity for crude oil reached 165 g g‑1, suggesting that VPRGS could be applied in oil leakage remediation. VPRGS could treat pollutants both in pure liquid form and in the simulated sea water, where the hydrophobic nature of VPRGS allowed the floating of VPRGS on simulated sea water. VPRGS could be easily regenerated without obvious capacity loss up to 9 cycles. The implications to the applications of VPRGS in oil/water separation and water remediation are discussed.

  3. Preparation of nanometer δ-and β-bismuth trioxide by vacuum vapor-phase oxidation

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    A stable δ- and β-bismuth trioxide was prepared at room temperature by vacuum vapor-phase oxidation. The average crystal size of products was 14.6 nm (by XRD), the d(0.5) value was in the range from 62 nm to 69 nm, and geometric standard deviation(GSD)was from 1.42 to 1.64. The results show that δ-Bi2O3 is formed when quenching rates is rapid and β-Bi2O3 is formed when it is slow. The size of grains increases with rising reaction temperature, flow rate of carrier gas, residual pressure of system and longer growing time of grains.

  4. Preparation,characterization and properties studies of quinine-imprinted polymer in the aqueous phase

    Institute of Scientific and Technical Information of China (English)

    He Jianfeng; Liu Lan; Yang Guilan; Deng Qinying

    2006-01-01

    The uniform-sized spherical molecularly imprinted polymers were successfully prepared through molecular imprinting technology by two-step seed swelling and mini-emulsion polymerization in the aqueous condition using quinine as template molecules and methacrylic acid (MAA)as functional monomer.The polymers were characterized by IR spectra,thermal-weight analysis,scanning electron microscope and laser particle size analysis.The properties of imprinted polymers were investigated in different organic phases and aqueous media.In the organic media,results suggested that polar interactions(hydrogen bonding,ionic interactions)between acidic monomer/polymer and template molecules are mainly responsible for the binding and recognition;whereas in the aqueous medium,a considerable recognition effect was also obtained where the ionic(electrostatic)interaction and hydrophobic interaction play an important role.The experiments of binding different substrates indicated that the MIPs possessed an excellent rebinding ability and inherent selectivity to quinine.

  5. The first preparative solution phase synthesis of melanotan II

    Directory of Open Access Journals (Sweden)

    2008-10-01

    Full Text Available Melanotan II is a synthetic cyclic heptapeptide used to prevent a sunlight-induced skin cancer by stimulating the skin tanning process. In this paper we report the first solution phase synthesis of the title compound. The hexapeptide sequence has been assembled by [(2+2+1+1] scheme. After removing the orthogonal protection, a carbodiimide mediated lactamization, involving the ε-amino group of lysine and γ-carboxy group of aspartic acid, led to a cyclic intermediate. Appending N-acetylnorleucine concluded the assembly of melanotan II molecule. Protection of the lateral groups in arginine and tryptophan was omitted for atom and step economy reasons. The total synthesis of melanotan II was accomplished in 12 steps with 2.6% overall yield, affording >90% pure peptide without using preparative chromatography.

  6. Preparation and evaluation of bonded linear polymethacrylate stationary phases for open tubular capillary electrokinetic chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Tan, Z.J.; Remcho, V.T. [West Virginia Univ., Morgantown, WV (United States)

    1997-02-15

    A new procedure for the preparation of thick polymethacrylate films bonded in 25 {mu}m i.d. fused-silica capillaries is developed. The etched silica surface is first modified with an unsaturated organosilane, which is later incorporated into the polymer film. The capillary is then filled with a monomer solution, and polymerization is initiated by incubation at elevated temperature. This thermoinitiation method enables the use of ordinary polyimide-jacketed capillaries in preparing the columns. The effect of monomer concentration on the resulting polymer film was studied by open tubular capillary electrokinetic chromatography using p-hydroxybenzoates (parabens) as test solutes. Good separations were achieved using short capillaries. Run-to-run retention time reproducibility was excellent, with RSDs of 2% (n = 50) being representative. For the linear polymer films produced, retention of analytes increased as the monomer concentration increased to a certain value, at which point the capacity factors level off with further increases in monomer concentration. The electroosmotic flow velocity decreases with increasing monomer concentration. The efficiency for an unretained test probe (acetone) reaches 270 000 plates/m. 13 refs., 10 figs., 1 tab.

  7. On-line comprehensive two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography for preparative isolation of Peucedanum praeruptorum.

    Science.gov (United States)

    Wang, Xin-Yuan; Li, Jia-Fu; Jian, Ya-Mei; Wu, Zhen; Fang, Mei-Juan; Qiu, Ying-Kun

    2015-03-27

    A new on-line comprehensive preparative two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography (2D NPLC × RPLC) system was developed for the separation of complicated natural products. It was based on the use of a silica gel packed medium-pressure column as the first dimension and an ODS preparative HPLC column as the second dimension. The two dimensions were connected with normal-phase (NP) and reversed-phase (RP) enrichment units, involving a newly developed airflow assisted adsorption (AAA) technique. The instrument operation and the performance of this NPLC × RPLC separation method were illustrated by gram-scale isolation of ethanol extract from the roots of Peucedanum praeruptorum. In total, 19 compounds with high purity were obtained via automated multi-step preparative separation in a short period of time using this system, and their structures were comprehensively characterized by ESI-MS, (1)H NMR, and (13)C NMR. Including two new compounds, five isomers in two groups with identical HPLC and TLC retention values were also obtained and identified by 1D NMR and 2D NMR. This is the first report of an NPLC × RPLC system successfully applied in an on-line preparative process. This system not only solved the interfacing problem of mobile-phase immiscibility caused by NP and RP separation, it also exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods.

  8. Preparation and Evaluation of Tretinoin Microemulsion Based on Pseudo-Ternary Phase Diagram

    Directory of Open Access Journals (Sweden)

    Fatemeh Leis

    2012-06-01

    Full Text Available Purpose: The aim of the present research was to formulate a transparent microemolsion as a topical delivery system for tretinoin for the treatment of acne. Methods: Microemulsion formulations prepared by mixing appropriate amount of surfactant including Tween 80 and Labrasol, co-surfactant such as propylene glycol (PG and oil phase including isopropyl myristate – transcutol P (10:1 ratio. The prepared microemolsions were evaluated regarding their particle size, zeta potential, conductivity, stability, viscosity, differential scanning calorimetry (DSC, scanning electron microscopy (SEM, refractory index (RI and pH. Results: The results showed that maximum oil was incorporated in microemolsion system that was contained surfactant to co-surfactant ratio (Km of 4:1. The mean droplets size range of microemulsion formulation were in the range of 14.1 to 36.5 nm and its refractory index (RI and pH were 1.46 and 6.1, respectively. Viscosity range was 200-350 cps. Drug release profile showed 49% of the drug released in the first 8 hours of experiment belong to ME-7. Also, Hexagonal and cubic structures were seen in the SEM photograph of the microemulsions. Conclusion: physicochemical properties and in vitro release were dependent upon the contents of S/C, water and, oil percentage in formulations.Also, ME-7 may be preferable for topical tretinoin formulation.

  9. Preparation of multi-locus DNA probe cocktail by liquid-phase reassociation.

    Science.gov (United States)

    Tamaki, Y; Fukuda, M; Kishida, T; Wang, W

    1995-08-01

    We developed a simple, rapid method for the preparation of a DNA-fingerprinting probe cocktail, and tested its usefulness in paternity testing. Exploiting the property of tandemly repetitive DNA segments to be rapidly renatured after heat denaturation, we enriched restriction fragments of a child's genomic DNA for minisatellites by liquid phase reassociation followed by capture with immobilized streptavidin. We amplified and simultaneously labeled the reassociation product by anchored PCR using a digoxigenin-labeling mixture. Using this probe cocktail, we were able to detect fingerprints of paternity case trios, and the results were corroborated by DNA fingerprinting with a commercially available probe as well as by conventional phenotyping. Our method enables one to prepare a fresh cocktail of probes from the DNA sample under study during the overnight electrophoresis and Southern transfer steps in DNA fingerprinting, and eliminates the need of having an expensive probe of limited shelf life. If one has a practical outlook on DNA fingerprinting and regard it as a preliminary test, one does not have to use a cloned DNA probe. The present study demonstrates that a multi-locus probe cocktail serves such a practical purpose.

  10. Preparation of ultrafiltration membrane by phase separation coupled with microwave irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Suryani, Puput Eka [Department of Chemical Engineering, Faculty of Engineering, Diponegoro University Jl. Prof. Soedarto, Semarang 50275, Central Java (Indonesia); Department of Chemical Engineering, Faculty of Engineering, UniversitasMuhammadiyah Surakarta Jl. Jendral Ahmad Yani, Surakarta 57102, Central Java (Indonesia); Purnama, Herry [Department of Chemical Engineering, Faculty of Engineering, UniversitasMuhammadiyah Surakarta Jl. Jendral Ahmad Yani, Surakarta 57102, Central Java (Indonesia); Susanto, Heru, E-mail: heru.susanto@undip.ac.id [Department of Chemical Engineering, Faculty of Engineering, Diponegoro University Jl. Prof. Soedarto, Semarang 50275, Central Java (Indonesia)

    2015-12-29

    Preparation of low fouling ultrafiltration membrane is still a big challenge in the membrane field. In this paper, polyether sulfone (PES) ultrafiltration membranes were prepared by non-solvent-induced phase separation (NIPS) coupled with microwave irradiation. Polyethylene glycol (PEG) and polyethylene glycol methacrylate (PEGMA) were used as additives to improve membrane hydrophilicity. In this study, the concentration of additive, irradiation time and microwave power was varied. The membranes were characterized by scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectroscopy, while the performances were tested by adsorptive and ultrafiltration fouling experiments. The results show that the irradiation time and irradiation power are very important parameter that influence the membrane characteristic. In addition, type and concentration of additive are other important parameters. The results suggest that microwave irradiation is the most important parameter influencing the membrane characteristic. Both pure water flux and fouling resistance increase with increasing irradiation time, power irradiation, and additive concentration. PES membrane with addition of 10% w/w PEG and irradiated by 130 W microwave power for 180 seconds is the best membrane performance.

  11. Classroom assessment of reading comprehension: How are preservice Foundation Phase teachers being prepared?

    Directory of Open Access Journals (Sweden)

    Carisma Nel

    2012-04-01

    Full Text Available A number of assessment studies in recent years have shown that the educational achievement of learners in South African schools is unacceptably poor. The Department of Education’s systemic evaluations, conducted in Grade 3 (first cycle in 2001, second cycle in 2007 show very low levels of literacy among learners. Reading comprehension and writing scores averaged 39% for the first and 36% for the second cycle. Research indicates that less attention has been given to children’s reading comprehension skills compared to decoding skills. Teacher preparation programmes should provide candidates with a rigorous, research-based curriculum and opportunities to practise a range of predefined skills and knowledge. The demands of competent literacy instruction and assessment, and the training experiences necessary to learn it, have been seriously underestimated by universities. Teacher education programmes should ensure that teachers, amongst other crucial aspects, know how to assess the progress of every student and change instruction when it is not working and also know how to communicate results of assessments to various stakeholders, especially parents. The purpose of this article is to report on the training that pre-service teachers receive, related to reading comprehension assessment practices, within a BEd foundation phase teacher preparation programme.

  12. Weakly doped InP layers prepared by liquid phase epitaxy using a modulated cooling rate

    Science.gov (United States)

    Krukovskyi, R.; Mykhashchuk, Y.; Kost, Y.; Krukovskyi, S.; Saldan, I.

    2017-04-01

    Epitaxial structures based on InP are widely used to manufacture a number of devices such as microwave transistors, light-emitting diodes, lasers and Gunn diodes. However, their temporary instability caused by heterogeneity of resistivity along the layer thickness and the influence of various external or internal factors prompts the need for the development of a new reliable technology for their preparation. Weak doping by Yb, Al and Sn together with modulation of the cooling rate applied to prepare InP epitaxial layers is suggested to be adopted within the liquid phase epitaxy (LPE) method. The experimental results confirm the optimized conditions created to get a uniform electron concentration in the active n-InP layer. A sharp profile of electron concentration in the n+-InP(substrate)/n-InP/n+-InP epitaxial structure was observed experimentally at the proposed modulated cooling rate of 0.3 °С-1.5 °С min-1. The proposed technological method can be used to control the electrical and physical properties of InP epitaxial layers to be used in Gunn diodes.

  13. [Nasal submicron emulsion of Scutellariae Radix extract preparation technology research based on phase transfer of solute technology].

    Science.gov (United States)

    Shi, Ya-jun; Shi, Jun-hui; Chen, Shi-bin; Yang, Ming

    2015-07-01

    Based on the demand of nasal drug delivery high drug loadings, using the unique phase transfer of solute, integrating the phospholipid complex preparation and submicron emulsion molding process of Scutellariae Radix extract, the study obtained the preparation of the high drug loadings submicron emulsion of Scutellariae Radix extract. In the study of drug solution dispersion method, the uniformity of drug dispersed as the evaluation index, the traditional mixing method, grinding, homogenate and solute phase transfer technology were investigated, and the solute phase transfer technology was adopted in the last. With the adoption of new technology, the drug loading capacity reached 1.33% (phospholipid complex was 4%). The drug loading capacity was improved significantly. The transfer of solute method and timing were studied as follows,join the oil phase when the volume of phospholipid complex anhydrous ethanol solution remaining 30%, the solute phase transfer was completed with the continued recycling of anhydrous ethanol. After drug dissolved away to oil phase, the preparation technology of colostrum was determined with the evaluation index of emulsion droplet form. The particle size of submicron emulsion, PDI and stability parameters were used as evaluation index, orthogonal methodology were adopted to optimize the submicron emulsion ingredient and main influential factors of high pressure homogenization technology. The optimized preparation technology of Scutellariae Radix extract nasal submicron emulsion is practical and stable.

  14. Preparation, characterization, and thermal properties of microencapsulated phase change material for thermal energy storage

    Energy Technology Data Exchange (ETDEWEB)

    Alkan, Cemil; Sari, Ahmet; Karaipekli, Ali [Department of Chemistry, Gaziosmanpasa University, 60240 Tokat (Turkey); Uzun, Orhan [Department of Physics, Gaziosmanpasa University, 60240 Tokat (Turkey)

    2009-01-15

    This study is focused on the preparation, characterization, and determination of thermal properties of microencapsulated docosane with polymethylmethacrylate (PMMA) as phase change material for thermal energy storage. Microencapsulation of docosane has been carried out by emulsion polymerization. The microencapsulated phase change material (MEPCM) was characterized using scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR) spectroscopy. Thermal properties and thermal stability of MEPCM were measured by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). DSC analysis indicated that the docosane in the microcapsules melts at 41.0 C and crystallizes at 40.6 C. It has latent heats of 54.6 and -48.7 J/g for melting and crystallization, respectively. TGA showed that the MEPCM degraded in three distinguishable steps and had good chemical stability. Accelerated thermal cycling tests also indicated that the MEPCM had good thermal reliability. Based on all these results, it can be concluded that the microencapsulated docosane as MEPCMs have good potential for thermal energy storage purposes such as solar space heating applications. (author)

  15. Monitoring preparation and phase transitions of carburized W(1 1 0) by reflectance difference spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Bachmann, Magdalena [Institute of Physical Chemistry, University of Innsbruck, Innrain 52a, A-6020 Innsbruck (Austria); Memmel, Norbert, E-mail: norbert.memmel@uibk.ac.at [Institute of Physical Chemistry, University of Innsbruck, Innrain 52a, A-6020 Innsbruck (Austria); Bertel, Erminald [Institute of Physical Chemistry, University of Innsbruck, Innrain 52a, A-6020 Innsbruck (Austria); Denk, Mariella; Hohage, Michael; Zeppenfeld, Peter [Institute of Experimental Physics, Johannes Kepler University Linz, Altenbergerstr. 69, A-4040 Linz (Austria)

    2012-10-01

    Highlights: Black-Right-Pointing-Pointer Real-time in situ monitoring of W(1 1 0) surface cleaning. Black-Right-Pointing-Pointer Real-time in situ monitoring of carburazation kinetics on W(1 1 0) by RDS. Black-Right-Pointing-Pointer Phase transformation R(15 Multiplication-Sign 3)-C/W(1 1 0)-R(15 Multiplication-Sign 12)-C/W(1 1 0) studied by RDS, AES and LEED. - Abstract: Reflectance difference spectroscopy (RDS) is applied to follow in situ the preparation of clean and carburized W(1 1 0) surfaces and to study the temperature-induced transition between the R(15 Multiplication-Sign 3) and R(15 Multiplication-Sign 12) carbon/tungsten surface phases. RDS data for this transition are compared to data obtained from Auger-electron spectroscopy and low-energy electron diffraction. All techniques reveal that this transition, occurring around 1870 K, is reversible with a small hysteresis, indicating a first-order-like behaviour. The present results also prove a high surface sensitivity of RDS, which is attributed to the excitation of electronic p-like surface resonances of W(1 1 0).

  16. Actuation behaviour of polyaniline films and tubes prepared by phase inversion technique

    Science.gov (United States)

    Xi, Binbin; Truong, Van-Tan; Mottaghitalab, Vahid; Whitten, Philip; Spinks, Geoffrey M.; Wallace, Gordon G.

    2005-02-01

    The phase inversion technique was used to produce polyaniline (PAn) actuators with different geometries that cannot be obtained by PAn cast from N-methyl-2-pyrrolidinone (NMP) solution in a conventional way. PAn was cast and coagulated in a water bath forming films and tubes with or without a platinum (Pt) wire helix as an interconnect. PAn was doped with hydrochloric solution (HCl, 1 M) (PAn/HCl) or methanesulfonic acid (MSA, 1 M) (PAn/MSA). In nitric acid (HNO3, 1 M) aqueous electrolyte, the actuation strain of PAn/HCl was 0.9% which increased to 2.0% and 2.7% for the tubes without and with the Pt helix, respectively. The Pt helix helped prevent the IR drop along the actuator. Comparing with NaNO3 (1 M) aqueous electrolyte, the use of HNO3 aqueous electrolyte gave better actuation stability where at least 100 cycles were observed and the final actuation strain was determined by the size of dopant. Change of coagulation bath from water to NMP (30% w/w)/water resulted in subtle difference in the Young"s modulus of PAn/MSA in oxidized and reduced states. PAn prepared by phase inversion technique is porous by nature, consequently it is brittle and exhibits a low actuation stress (0.3 - 0.4 MPa).

  17. Actuation behaviour of polyaniline films and tubes prepared by the phase inversion technique

    Science.gov (United States)

    Xi, Binbin; Truong, Van-Tan; Mottaghitalab, Vahid; Whitten, Philip G.; Spinks, Geoffrey M.; Wallace, Gordon G.

    2007-10-01

    The phase inversion technique was used to produce polyaniline (PAn) actuators with film and tube geometries. PAn dissolved in N,N-dimethyl propylene urea was cast, and then coagulated in a water bath forming films and tubes with and without a platinum (Pt) wire helix as an interconnect. The solid PAn was doped with hydrochloric acid solution (1 M HCl) (PAn/HCl) or methanesulfonic acid (1 M MSA) (PAn/MSA). The actuation strain was observed in different electrolytes using constant current stimulation at a frequency of 1 pulse per minute. In nitric acid (1 M HNO3) electrolyte, the actuation strain produced by the PAn/HCl film was 0.9%. The strain increased to 2.0% and 2.7% when the actuator geometry was changed to tube, then to tube with a Pt helix, respectively. Compared to 1 M NaNO3 electrolyte, the use of 1 M HNO3 electrolyte gave better actuation stability, where more than 100 cycles were observed. Changing the coagulation bath from water to NMP (30% w/w)/water resulted in a subtle difference in the Young's modulus of PAn/MSA in the oxidized and reduced states. PAn prepared by the phase inversion technique was porous by nature; consequently it is brittle and exhibits a low actuation stress (400 kPa).

  18. Study on preparation and application of novel saponification agent for organic phase of rare earths extraction

    Institute of Scientific and Technical Information of China (English)

    FENG Zongyu; HUANG Xiaowei; LIU Hongji; WANG Meng; LONG Zhiqi; YU Ying; WANG Chunmei

    2012-01-01

    In view of the problem of ammonia-nitrogen wastewater pollution in rare earths extraction and separation,the novel saponification agent of organic phase,which is magnesium bicarbonate solution,was prepared with the natural rich and cheap dolomite as mw material through carbonation process.The behavior and purification of main impurities ions in the carbonation process as well as the application effect of the novel saponification agent in the extraction and separation was researched.The results showed that the concentration of Fe,Al,Si impurities ions was.less than 5 ppm in the saponification agent through the development of effective removal technology,respectively.When the novel saponification agent was used in the extraction and separation,magnesium utilization rote was more than 95%,and rare earths extraction rate above 99.5% has achieved.Therefore,the technology could replace ammonia-water to saponify the organic phase in rare earth extraction and separation process.

  19. Silicate-entrapped porous coatings for preparing high-efficiency solid-phase microextraction sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Breton, Francois; Monton, Maria Rowena N. [University of Waterloo, Department of Chemistry, 200 University Ave. West, Waterloo, Ontario N2L 3G1 (Canada); Mullett, Wayne M. [MDS Nordion, 447 Marsh Road, Ottawa, Ontario K2K 1X8 (Canada); Pawliszyn, Janusz, E-mail: janusz@uwaterloo.ca [University of Waterloo, Department of Chemistry, 200 University Ave. West, Waterloo, Ontario N2L 3G1 (Canada)

    2010-06-11

    We present a novel way to prepare SPME fibers using a silicate entrapment of porous particles, followed by derivatization using classical organosilane chemistry. The fibers provide a good platform for on-fiber derivatization of desired extraction phases while providing porosity necessary for high extractions capacities. The porous network was created using potassium silicate and porous silica particles. Fibers derivatized using n-butyl, n-octyl, n-octadecyl and n-triacontyl groups were shown to extract benzodiazepines successfully. The coatings were determined to have an average thickness of ca. 8 {mu}m, as determined by a scanning electron microscope, permitting equilibrium times as fast as 2 min. The fibers also showed very good ruggedness towards a vast range of solvents and prolonged use. It was determined that greater extraction efficiencies could be obtained using triacontyl as an extraction phase. The C18 and C30 fibers were also found to provide good linearity (>0.99) for the model analytes over two orders of magnitude, with limits of detection in the sub ng mL{sup -1} levels. C30 fibers were used to establish a correlation between structurally diverse {beta}-blockers and their literature reported Log P values. The C30 fibers provided a good correlation (R{sup 2} = 0.9255) between {beta}-blockers ranging in hydrophobicity from Log P{sub literature} 0.16-4.15 and their respective experimentally determined Log K{sub spme} values.

  20. Advanced fabrication method for the preparation of MOF thin films: Liquid-phase epitaxy approach meets spin coating method.

    KAUST Repository

    Chernikova, Valeriya

    2016-07-14

    Here we report a new and advanced method for the fabrication of highly oriented/polycrystalline metal-organic framework (MOF) thin films. Building on the attractive features of the liquid-phase epitaxy (LPE) approach, a facile spin coating method was implemented to generate MOF thin films in a high-throughput fashion. Advantageously, this approach offers a great prospective to cost-effectively construct thin-films with a significantly shortened preparation time and a lessened chemicals and solvents consumption, as compared to the conventional LPE-process. Certainly, this new spin-coating approach has been implemented successfully to construct various MOF thin films, ranging in thickness from a few micrometers down to the nanometer scale, spanning 2-D and 3-D benchmark MOF materials including Cu2(bdc)2•xH2O, Zn2(bdc)2•xH2O, HKUST-1 and ZIF-8. This method was appraised and proved effective on a variety of substrates comprising functionalized gold, silicon, glass, porous stainless steel and aluminum oxide. The facile, high-throughput and cost-effective nature of this approach, coupled with the successful thin film growth and substrate versatility, represents the next generation of methods for MOF thin film fabrication. Thereby paving the way for these unique MOF materials to address a wide range of challenges in the areas of sensing devices and membrane technology.

  1. Advanced Fabrication Method for the Preparation of MOF Thin Films: Liquid-Phase Epitaxy Approach Meets Spin Coating Method.

    Science.gov (United States)

    Chernikova, Valeriya; Shekhah, Osama; Eddaoudi, Mohamed

    2016-08-10

    Here, we report a new and advanced method for the fabrication of highly oriented/polycrystalline metal-organic framework (MOF) thin films. Building on the attractive features of the liquid-phase epitaxy (LPE) approach, a facile spin coating method was implemented to generate MOF thin films in a high-throughput fashion. Advantageously, this approach offers a great prospective to cost-effectively construct thin-films with a significantly shortened preparation time and a lessened chemicals and solvents consumption, as compared to the conventional LPE-process. Certainly, this new spin-coating approach has been implemented successfully to construct various MOF thin films, ranging in thickness from a few micrometers down to the nanometer scale, spanning 2-D and 3-D benchmark MOF materials including Cu2(bdc)2·xH2O, Zn2(bdc)2·xH2O, HKUST-1, and ZIF-8. This method was appraised and proved effective on a variety of substrates comprising functionalized gold, silicon, glass, porous stainless steel, and aluminum oxide. The facile, high-throughput and cost-effective nature of this approach, coupled with the successful thin film growth and substrate versatility, represents the next generation of methods for MOF thin film fabrication. Therefore, paving the way for these unique MOF materials to address a wide range of challenges in the areas of sensing devices and membrane technology.

  2. A new generation of more pH stable reversed phases prepared by silanization of zirconized silica.

    Science.gov (United States)

    Silva, César R; Airoldi, Claudio; Collins, Kenneth E; Collins, Carol H

    2008-05-16

    To further extend our studies in the search for reversed phases with enhanced durability at high pH, zirconized silica has now been explored as an alternative support. The synthesis of the new stationary phases involves silanization of a zirconium-modified silica support with a C(18) trifunctional silane, followed by endcapping. The chromatographic properties of the C(18) phases based on zirconized silica are similar to their titanized silica counterparts. Accelerated high pH stability tests, using phosphate mobile phases and elevated temperature, have shown that the zirconized silica phases have promising advantages not only over similarly prepared non-metalized phases but also over titanized silica C(18) phases.

  3. Exploring Feasibility for Application of Luminescent CdTe Quantum Dots Prepared in Aqueous Phase to Live Cell Imaging

    Institute of Scientific and Technical Information of China (English)

    Ji Fang WENG; Xing Tao SONG; Liang LI; Hui Feng QIAN; Ke Ying CHEN; Xue Ming XU; Cheng Xi CAO; Ji Cun REN

    2006-01-01

    This paper explored the feasibility for the application of luminescent CdTe quantum dots prepared in aqueous phase to live cell imaging. The highly luminescent CdTe quantum dots (QDs)were first prepared in aqueous phase, and then were covalently coupled to a plant lectin (UEA-1),as a fluorescent probe. After incubating with of human umbilical vein endothelial cells (HUVECs), the QD probe with UEA-1 was able to specifically bind the corresponding cell receptor. The good cell images were obtained in live cells using laser confocal scanning microscopy. We predict that QDs prepared in water phase will probably become an attractive alternative probe in cellular imaging and bio-labeling.

  4. 信息动态%Preparation of Polysaccharide Derivatives-based Composite Chiral Stationary Phases and Their Chiral Recognition

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    Two coated-type composite chiral stationary phases (CSPs) were prepared based on cellulose tris(3,5-dimethylphenylcarbamate) (CDMPC) and amylose tris (3,5-dimethylphenylcarbamate)(ADMPC) by coating the corresponding derivatives onto 3-aminopropyl silica gel separately and then mixing or by coating the mixed derivatives onto silica gel. The CSPs containing only CDMPC or ADMPC were also prepared for comparison. The mixing method does not significantly influence the enantioselectivities. The composite CSPs generally show chiral recognition abilities intermediate between those of the two individual phases, while some racemates were poorer and at the same time one was better resolved on the composite CSPs.

  5. Preparation and Evaluation of a Novel Cellulose Tris(N-3,5-dimethylphenylcarbamate) Chiral Stationary Phase

    Institute of Scientific and Technical Information of China (English)

    GE,Jin; ZHAO,Liang; SHI,Yan-Ping

    2008-01-01

    A novel cellulose tris(N-3,5-dimethylphenylcarbamate) (CDMPC) chiral stationary phase (CSP) was prepared by coating CDMPC on TiO2/SiO2, which was prepared by coating titania nanoparticles on silica through a self-assemble technique. At first, 2-hydroxyl-phenyl acetonitrile and α-phenylethanol were separated on this new CSP to evaluate the chiral separation ability. Then, two pesticides, matalaxyl and diclofop-methyl were separated.The influence of the mobile phase composition on the enantioselectivity was discussed, and the repeatability and stability of the CSP were studied too.

  6. Preparation and thermal energy storage properties of paraffin/calcined diatomite composites as form-stable phase change materials

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Zhiming [School of Chemical and Environmental Engineering, China University of Mining and Technology, Beijing 100083 (China); Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Zhang, Yuzhong [School of Chemical and Environmental Engineering, China University of Mining and Technology, Beijing 100083 (China); Zheng, Shuilin, E-mail: shuilinzh@yahoo.com.cn [School of Chemical and Environmental Engineering, China University of Mining and Technology, Beijing 100083 (China); Park, Yuri [Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Frost, Ray L., E-mail: r.frost@qut.edu.au [Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane, Queensland 4001 (Australia)

    2013-04-20

    Highlights: ► Composite phase change material (PCM) was prepared by blending composite paraffin and calcined diatomite. ► The optimum mixed proportion was obtained through differential scanning calorimetry. ► Thermal energy storage properties of the composite PCMs were determined by DSC. ► Thermal cycling test showed that the prepared PCMs are thermally reliable and chemically stable. - Abstract: A composite paraffin-based phase change material (PCM) was prepared by blending composite paraffin and calcined diatomite through the fusion adsorption method. In this study, raw diatomite was purified by thermal treatment in order to improve the adsorption capacity of diatomite, which acted as a carrier material to prepare shape-stabilized PCMs. Two forms of paraffin (paraffin waxes and liquid paraffin) with different melting points were blended together by the fusion method, and the optimum mixed proportion with a suitable phase-transition temperature was obtained through differential scanning calorimetry (DSC) analysis. Then the prepared composite paraffin was adsorbed in calcined diatomite. The prepared paraffin/calcined diatomite composites were characterized by the scanning electron microscope (SEM) and Fourier transformation infrared (FT-IR) analysis techniques. Thermal energy storage properties of the composite PCMs were determined by DSC method. DSC results showed that there was an optimum adsorption ratio between composite paraffin and calcined diatomite and the phase-transition temperature and the latent heat of the composite PCMs were 33.04 °C and 89.54 J/g, respectively. Thermal cycling test of composite PCMs showed that the prepared material is thermally reliable and chemically stable. The obtained paraffin/calcined diatomite composites have proper latent heat and melting temperatures, and show practical significance and good potential application value.

  7. Preparation and Characterization of Microencapsulated Phase Change Materials for Use in Building Applications

    Directory of Open Access Journals (Sweden)

    Jessica Giro-Paloma

    2015-12-01

    Full Text Available A method for preparing and characterizing microencapsulated phase change materials (MPCM was developed. A comparison with a commercial MPCM is also presented. Both MPCM contained paraffin wax as PCM with acrylic shell. The melting temperature of the PCM was around 21 °C, suitable for building applications. The M-2 (our laboratory made sample and Micronal® DS 5008 X (BASF samples were characterized using SEM, DSC, nano-indentation technique, and Gas Chromatography/Mass spectrometry (GC-MS. Both samples presented a 6 μm average size and a spherical shape. Thermal energy storage (TES capacities were 111.73 J·g−1 and 99.3 J·g−1 for M-2 and Micronal® DS 5008 X, respectively. Mechanical characterization of the samples was performed by nano-indentation technique in order to determine the elastic modulus (E, load at maximum displacement (Pm, and displacement at maximum load (hm, concluding that M-2 presented slightly better mechanical properties. Finally, an important parameter for considering use in buildings is the release of volatile organic compounds (VOC’s. This characteristic was studied at 65 °C by CG-MS. Both samples showed VOC’s emission after 10 min of heating, however peaks intensity of VOC’s generated from M-2 microcapsules showed a lower concentration than Micronal® DS 5008 X.

  8. Superhydrophilic porous TiO 2 film prepared by phase separation through two stabilizers

    Science.gov (United States)

    Huang, Weixin; Deng, Wei; Lei, Ming; Huang, Hong

    2011-03-01

    A novel method was developed to produce a TiO 2 film with circular pores on its surface. The pores aroused from the precursor solution using both acetylacetone (AcAc) and diethanolamine (DEA) as stabilizers. The appearance of interconnected or isolated pores for the films was discussed in relation to the phase separation in the sol-gel process with the presence of Acac and DEA. Macropore size, together with connectivity of pores and gel skeleton, can be controlled by selecting an appropriate composition for preparation at DEA amount or regulating a time scale of the sol-gel transition. Finally, wetting behavior of the resulting films was characterized by using contact angle measurements. The TiO 2 films with interconnected or relatively isolated pores exhibit superhydrophilic characteristic, although it is not exposed to ultraviolet irradiation. Deducing from the Wenzel-Cassie regimes' transition criterion, the existence of Cassie impregnating wetting regime rather than Wenzel one upon these porosity-driven superhydrophilic surfaces can be obtained.

  9. Preparation by a Rheological Phase Reaction Method and Thermal Decomposition Reaction Mechanism of Nickelous Salicylate Tetrahydrate

    Institute of Scientific and Technical Information of China (English)

    WangJin-long; YuanLiang-jie; YangYi-yong; SunJu-tang; ZhangKe-li

    2003-01-01

    The single crystal nickel salicylate tetrahydrate was prepared with the rheological phase reaction method from nickelous hydroxide and salicylic acid. The crystal structure was determinecL It is monoclinic, space group P21/n, α=0.678 74(3), b=0. 515 91(2), c=2. 313 30(9) nm, β=90.9286(17)°,V=0. 809 94(6) nm3, Z=2, ρcalod =1. 661 g· cm-3. Final R indices: R=0. 027 9 and ωR=0.065 0[Ⅰ>2σ(Ⅰ)]. The thermal decomposition mechanism in an inert atmosphere was investigated via TG, DTG and DTA. The thermal decomposition products were characterized with IR and micro-powder X-ray diffraction method. A new coordination polymer ( NiC6 H4 O)n as an intermediate product and nanoscale metal nickel were obtained in the ranges of 364-429℃ and 429-680℃, respectively.

  10. Preparation and crystalline phase of a TiO2 porous film by anodic oxidation

    Institute of Scientific and Technical Information of China (English)

    WANG Wei; TAO Jie; ZHANG Weiwei; TAO Haijun; WANG Ling

    2005-01-01

    Anatase titanium dioxide is an active photocatalyst, but it is difficult to immobilize on the substrate. A crystalline TiO2 porous film was prepared directly on the surface of pure titanium by anodic oxidation in this work. Constant voltage and constant current anodic oxidation were adopted with sulphuric acid used as the electrolyte, pure titanium as the anode and copper as the cathode. The morphology and structure of the porous film on the substrate were analyzed with the aid of Field Emission Scanning Electron Microscopy (FESEM) and X-ray Diffraction (XRD). The effects of the parameters of anodic oxidation (such as voltage, the concentration of sulphuric acid, anodization time and current density) on the aperture and the crystalline phase of the TiO2 porous film were systematically investigated. The results indicate that the increase of current density facilitates the augment of the aperture and the generation of anatase and rutile. In addition, the forming mechanism of anatase and rutile TiO2 porous films was discussed.

  11. Preparation and characterization of porous carbon material-coated solid-phase microextraction metal fibers.

    Science.gov (United States)

    Zhu, Fang; Guo, Jiaming; Zeng, Feng; Fu, Ruowen; Wu, Dingcai; Luan, Tiangang; Tong, Yexiang; Lu, Tongbu; Ouyang, Gangfeng

    2010-12-10

    Two kinds of porous carbon materials, including carbon aerogels (CAs), wormhole-like mesoporous carbons (WMCs), were synthesized and used as the coatings of solid-phase microextraction (SPME) fibers. By using stainless steel wire as the supporting core, six types of fibers were prepared with sol-gel method, direct coating method and direct coating plus sol-gel method. Headspace SPME experiments indicated that the extraction efficiencies of the CA fibers are better than those of the WMC fibers, although the surface area of WMCs is much higher than that of CAs. The sol-gel-CA fiber (CA-A) exhibited excellent extraction properties for non-polar compounds (BTEX, benzene, toluene, ethylbenzene, o-xylene), while direct-coated CA fiber (CA-B) presented the best performance in extracting polar compounds (phenols). The two CA fibers showed wide linear ranges, low detection limits (0.008-0.047μgL(-1) for BTEX, 0.15-5.7μgL(-1) for phenols) and good repeatabilities (RSDs less than 4.6% for BTEX, and less than 9.5% for phenols) and satisfying reproducibilities between fibers (RSDs less than 5.2% for BTEX, and less than 9.9% for phenols). These fibers were successfully used for the analysis of water samples from the Pearl River, which demonstrated the applicability of the home-made CA fibers.

  12. Graphene nanoplatelets-reinforced polyetherimide foams prepared by water vapor-induced phase separation

    Directory of Open Access Journals (Sweden)

    H. Abbasi

    2015-05-01

    Full Text Available The present work considers the preparation of medium-density polyetherimide foams reinforced with variable amounts of graphene nanoplatelets (1–10 wt% by means of water vapor-induced phase separation (WVIPS and their characterization . A homogeneous closed-cell structure with cell sizes around 10 µm was obtained, with foams exhibiting zero crystallinity according to X-ray diffraction (XRD. Thermogravimetric analysis under nitrogen showed a two-step thermal decomposition behaviour for both unfilled and graphene-reinforced foams, with foams containing graphene presenting thermal stability improvements, related to a physical barrier effect promoted by the nanoplatelets. Thermo-mechanical analysis indicated that the specific storage modulus of the nanocomposite foams significantly increased owing to the high stiffness of graphene and finer cellular morphology of the foams. Although foamed nanocomposites displayed no further sign of graphene nanoplatelets exfoliation, the electrical conductivity of these foams was significant even for low graphene contents, with a tunnel-like model fitting well to the evolution of the electrical conductivity with the amount of graphene.

  13. Graphenized pencil lead fiber: facile preparation and application in solid-phase microextraction.

    Science.gov (United States)

    Liu, Qian; Cheng, Mengting; Long, Yanmin; Yu, Miao; Wang, Thanh; Jiang, Guibin

    2014-01-17

    Graphenized pencil lead fiber was facilely prepared by in situ chemical exfoliation of graphite in pencil lead fiber to few-layered graphene sheets via a one-pot, one-step pressurized oxidation reaction for the first time. This new fiber was characterized and demonstrated to be a highly efficient but low-cost solid-phase microextraction (SPME) fiber. The extraction performance of the fiber was evaluated with four bisphenol analogs [bisphenol A (BPA), bisphenol S (BPS), bisphenol AF (BPAF), and tetrabromobisphenol A (TBBPA)] as model analytes in direct SPME mode. Unlike commercially available fibers, the graphenized pencil lead fiber showed an excellent chemical stability in highly saline, acidic, alkaline and organic conditions due to its coating-free configuration. The fiber also showed a very long lifespan. Furthermore, high extraction efficiency and good selectivity for the analytes with a wide polarity range could be obtained due to the exceptional properties of graphene. The detection limits (LODs) for the analytes were in the range of 1.1-25ng/L. The fiber was successfully applied in the analysis of tap water and effluent samples from a waste water treatment plant with spike recoveries ranging from 68.5 to 105.1%. Therefore, the graphenized pencil lead fiber provides a high performance, cheap, robust, and reliable tool for SPME.

  14. [Preparation and application of solid phase extraction packing of zirconia microsphere coated with sulfonated crosslinked polystyrene].

    Science.gov (United States)

    Shen, Shuchang; Liu, Yuhui; Xiao, Xiaoxing

    2013-08-01

    Zirconia microsphere was prepared by polymerization-induced colloid aggregation (PICA) method and carbon-carbon double bond was grafted onto its surface by titanic acid ester coupling reagent. Poly(styrene-divinylbenzene) was synthesized by free radical polymerization by using styrene, divinylbenzene and carbon-carbon double bond on the microsphere surface in solution system, so the polymer was coated on the microsphere surface. After the benzene ring of the polymer was sulfonated, the cation exchange packing for solid phase extraction (SPE) was obtained. The material was characterized by Fourier transform infrared spectroscopy, scanning electron microscope and X-ray energy dispersive spectroscopy. Three herbicides of mesotrione, atrazine and acetochlor in water were determined by the SPE cartridge coupled with high performance liquid chromatography (HPLC). In the range of 0.5 - 3.0 mg/L, the relationships between the peak areas and mass concentrations of mesotrione, atrazine and acetochlor were linear with the correlation coefficients of 0.9936, 0.9925, 0.9919, respectively. The limits of detection were 5.41, 6.72 and 13.4 microg/L for mesotrione, atrazine and acetochlor, respectively. The results showed that the zirconium dioxide microspheres coated with polymer have diameters in the range of about 6 to 8 microm, the SPE cartridges of which have high adsorption rate for the targets.

  15. Design and Preparation of Carbon Based Composite Phase Change Material for Energy Piles

    Directory of Open Access Journals (Sweden)

    Haibin Yang

    2017-04-01

    Full Text Available Energy piles—A fairly new renewable energy concept—Use a ground heat exchanger (GHE in the foundation piles to supply heating and cooling loads to the supported building. Applying phase change materials (PCMs to piles can help in maintaining a stable temperature within the piles and can then influence the axial load acting on the piles. In this study, two kinds of carbon-based composite PCMs (expanded graphite-based PCM and graphite nanoplatelet-based PCM were prepared by vacuum impregnation for potential application in energy piles. Thereafter, a systematic study was performed and different characterization tests were carried out on two composite PCMs. The composite PCMs retained up to 93.1% of paraffin and were chemically compatible, thermally stable and reliable. The latent heat of the composite PCM was up to 152.8 J/g while the compressive strength of cement paste containing 10 wt % GNP-PCM was found to be 37 MPa. Hence, the developed composite PCM has potential for thermal energy storage applications.

  16. Preparation of shape-stabilized phase change materials as temperature-adjusting powder

    Institute of Scientific and Technical Information of China (English)

    MIAO Chunyan; L(U) Gang; YAO Youwei; TANG Guoyi; WENG Duan

    2007-01-01

    The shape-stabilized phase change materials (PCMs)composed of paraffin wax and silica were prepared in O/W emulsion with cetyl trimethylamine bromide as emulsifier and n-pentanol as assist emulsifier.The paraffin wax(with melting temperature of 29℃,crystallizing temperature of 26℃ and latent heat of 142 J/g)served as latent heat storage material and the silica as supporting material,which prevented the leakage of the melted paraffin wax.Silica supporting material was formed in situ via hydrolysis and condensation from low-cost sodium silicate solution with chlorhydric acid and ammonium bicarbonate as neutralizing agent.The thermogravimetry(TG)curves show that the composite has a thermal stability superior to that of paraffin wax and that the content of paraffin wax in the composite is 65wt%.The maximum latent heat and its relevant melting point of composite are 95 J/g and 30℃,respectively.

  17. Preparation of microcrystals in lipidic cubic phase for serial femtosecond crystallography.

    Science.gov (United States)

    Liu, Wei; Ishchenko, Andrii; Cherezov, Vadim

    2014-09-01

    We have recently established a procedure for serial femtosecond crystallography (SFX) in lipidic cubic phase (LCP) for protein structure determination at X-ray free-electron lasers (XFELs). LCP-SFX uses the gel-like LCP as a matrix for growth and delivery of membrane protein microcrystals for crystallographic data collection. LCP is a liquid-crystalline mesophase composed of lipids and water. It provides a membrane-mimicking environment that stabilizes membrane proteins and supports their crystallization. Here we describe detailed procedures for the preparation and characterization of microcrystals for LCP-SFX applications. The advantages of LCP-SFX over traditional crystallographic methods include the capability of collecting room-temperature high-resolution data with minimal effects of radiation damage from sub-10-μm crystals of membrane and soluble proteins that are difficult to crystallize, while eliminating the need for crystal harvesting and cryo-cooling. Compared with SFX methods for microcrystals in solution using liquid injectors, LCP-SFX reduces protein consumption by 2-3 orders of magnitude for data collection at currently available XFELs. The whole procedure typically takes 3-5 d, including the time required for the crystals to grow.

  18. Phase change Materials (PCM) microcapsules with different shell compositions: Preparation, characterization and thermal stability

    Energy Technology Data Exchange (ETDEWEB)

    Bayes-Garcia, L.; Ventola, L.; Cordobilla, R.; Benages, R.; Calvet, T.; Cuevas-Diarte, M.A. [Departament de Cristal.lografia, Mineralogia i Diposits Minerals, Facultat de Geologia, Universitat de Barcelona, Marti i Franques s/n, E-08028 Barcelona (Spain)

    2010-07-15

    In this study, phase change materials (Rubitherm registered RT 27) microcapsules were successfully obtained by two different methods. The main difference between them remains on the shell composition, as they are composed of different coacervates (Sterilized Gelatine/Arabic Gum for the SG/AG method and Agar-Agar/Arabic Gum for the AA/AG method). Microcapsules were thermally characterized by thermo-optical microscopy and differential scanning calorimetry. Using scanning electron microscopy, their spherical morphology (sphericity factor of 0.94-0.95) and their particle size distribution were determined, obtaining an average diameter of 12 {mu}m for the SG/AG method and lower values for the AA/AG method, where nanocapsules were also observed (average diameter of 4.3 {mu}m for the microcapsules and 104 nm for the nanocapsules). The thermal stability determination was carried out by Thermogravimetric analyses (TG) and the results show a high decomposition temperature, although the process takes places in four steps for the two mentioned methods. Moreover, the microcapsules obtained by the AA/AG method decompose in a more gradual way, as in the TG results a double step, instead of one, is appreciable. On the whole, the prepared microencapsulated PCM are totally capable of developing their role in thermal energy storage. (author)

  19. Compact, Programmable, and Stable Biofunctionalized Upconversion Nanoparticles Prepared through Peptide-Mediated Phase Transfer for High-Sensitive Protease Sensing and in Vivo Apoptosis Imaging.

    Science.gov (United States)

    Zeng, Tao; Zhang, Tao; Wei, Wei; Li, Zhi; Wu, Dan; Wang, Li; Guo, Jun; He, Xuewen; Ma, Nan

    2015-06-10

    Protease represents an important class of biomarkers for disease diagnostics and drug screening. Conventional fluorescence-based probes for in vivo protease imaging suffer from short excitation wavelengths and poor photostability. Upconversion nanoparticles (UCNPs) hold great promise for biosensing and bioimaging because of their deep-tissue excitability, robust photostability, and minimal imaging background. However, producing highly stable and compact biofunctionalized UCNP probes with optimal bioresponsivity for in vivo imaging of protease activities still remains challenging and has not been previously demonstrated. Herein, we report facile preparation of highly compact and stable biofunctionalized UCNPs through peptide-mediated phase transfer for high-sensitive detection of protease in vitro and in vivo. We demonstrate that the polyhistidine-containing chimeric peptides could displace oleic acid molecules capped on UCNPs synthesized in organic solvents and, thereby, directly transfer UCNPs from the chloroform phase to the water phase. The resulting UCNPs possess high stability, programmable surface properties, and a compact coating layer with minimized thickness for efficient luminescence resonance energy transfer (LRET). On the basis of this strategy, we prepared LRET-based UCNP probes with optimal bioresponsivity for in vitro high-sensitive detection of trypsin and in vivo imaging of apoptosis for chemotherapy efficacy evaluation. The reported strategy could be extended to construct a variety of peptide-functionalized UCNPs for various biomedical applications.

  20. Preparation, characterization, and thermal properties of starch microencapsulated fatty acids as phase change materials thermal energy storage applications

    Science.gov (United States)

    Stable starch-oil composites can be prepared from renewable resources by excess steam jet-cooking aqueous slurries of starch and vegetable oils or other hydrophobic materials. Fatty acids such as stearic acid are promising phase change materials (PCMs) for latent heat thermal energy storage applica...

  1. Representing dispositions

    Directory of Open Access Journals (Sweden)

    Röhl Johannes

    2011-08-01

    Full Text Available Abstract Dispositions and tendencies feature significantly in the biomedical domain and therefore in representations of knowledge of that domain. They are not only important for specific applications like an infectious disease ontology, but also as part of a general strategy for modelling knowledge about molecular interactions. But the task of representing dispositions in some formal ontological systems is fraught with several problems, which are partly due to the fact that Description Logics can only deal well with binary relations. The paper will discuss some of the results of the philosophical debate about dispositions, in order to see whether the formal relations needed to represent dispositions can be broken down to binary relations. Finally, we will discuss problems arising from the possibility of the absence of realizations, of multi-track or multi-trigger dispositions and offer suggestions on how to deal with them.

  2. Hierarchical Porous Polymer Beads Prepared by Polymerization-induced Phase Separation and Emulsion-template in a Microfluidic Device

    Institute of Scientific and Technical Information of China (English)

    Wei-cai Wang; Yan-xiong Pan; Kai Shi; Chao Peng; Xiang-ling Ji

    2014-01-01

    Porous polymer beads (PPBs) containing hierarchical bimodal pore structure with gigapores and meso-macropores were prepared by polymerization-induced phase separation (PIPS) and emulsion-template technique in a glass capillary microfluidic device (GCMD).Fabrication procedure involved the preparation of water-in-oil emulsion by emulsifying aqueous solution into the monomer solution that contains porogen.The emulsion was added into the GCMD to fabricate the (water-in-oil)-in-water double emulsion droplets.The flow rate of the carrier continuous phase strongly influenced the formation mechanism and size of droplets.Formation mechanism transformed from dripping to jetting and size of droplets decreased from 550 μm to 250 μm with the increase in flow rate of the carrier continuous phase.The prepared droplets were initiated for polymerization by on-line UV-irradiation to form PPBs.The meso-macropores in these beads were generated by PIPS because of the presence ofporogen and gigapores obtained from the emulsion-template.The pore morphology and pore size distribution of the PPBs were investigated extensively by scanning electron microscopy and mercury intrusion porosimetry (MIP).New pore morphology was formed at the edge of the beads different from traditional theory because of different osmolarities between the water phase of the emulsion and the cartier continuous phase.The morphology and proportion of bimodal pore structure can be tuned by changing the kind and amount of porogen.

  3. Preparation of the multienzyme system gramicidin S-synthetase 2 with an aqueous three-phase system.

    Science.gov (United States)

    Kirchner, A; Simonis, M; von Döhren, H

    1987-06-19

    The distribution of gramicidin S-synthetase activity from disrupted cells suspended in aqueous two- and three-phase systems was investigated. An optimized three-phase system containing 5% dextran, 8% Ficoll, 11% PEG and 6.7% disrupted cells was found to be effective in extracting gramicidin S-synthetase activity. The activity yield achieved was higher in comparison to other preparation methods, and the subsequent purification steps were greatly facilitated. The time needed for the preparation of the labile gramicidin S-synthetase was considerably reduced. The combination of the aqueous phase extraction with chromatographic methods yielded 19 mg gramicidin S-synthetase 2 in essentially pure form from 30 g (wet weight) of cells.

  4. Preparation of a novel carboxyl stationary phase by "thiol-ene" click chemistry for hydrophilic interaction chromatography.

    Science.gov (United States)

    Peng, Xi-Tian; Liu, Tao; Ji, Shu-Xian; Feng, Yu-Qi

    2013-08-01

    A novel carboxyl-bonded silica stationary phase was prepared by "thiol-ene" click chemistry. The resultant Thiol-Click-COOH phase was evaluated under hydrophilic interaction liquid chromatography (HILIC) mobile phase conditions. A comparison of the chromatographic performance of Thiol-Click-COOH and pure silica columns was performed according to the retention behaviors of analytes and the charged state of the stationary phases. The results indicated that the newly developed Thiol-Click-COOH column has a higher surface charge and stronger hydrophilicity than the pure silica column. Furthermore, the chromatographic behaviors of five nucleosides on the Thiol-Click-COOH phase were investigated in detail. Finally, a good separation of 13 nucleosides and bases, and four water-soluble vitamins was achieved.

  5. Preparation and photocatalytic activity of bicrystal phase TiO2 nanotubes containing TiO2-B and anatase

    Science.gov (United States)

    Huang, Chuanxi; Zhu, Kerong; Qi, Mengyao; Zhuang, Yonglong; Cheng, Chao

    2012-06-01

    Bicrystal phase TiO2 nanotubes (NTS) containing monoclinic TiO2-B and anatase were prepared by the hydrothermal reaction of anatase nanoparticles with NaOH aqueous solution and a heat treatment. Their structure was characterized by XRD, TEM and Raman spectra. The results showed that the bicrystal phase TiO2 NTS were formed after calcining H2Ti4O9·H2O NTS at 573 K. The bicrystal phase TiO2 NTS exhibit significantly higher photocatalytic activity than the single phase anatase NTS and Dessuga P-25 nanoparticles in the degradation of Methyl Orange aqueous solution under ultraviolet light irradiation, which is attributed to the large surface and interface areas of the bicrystal phase TiO2 NTS.

  6. [Preparation of weak light driven TiO2 multi composite photocatalysts via adsorption phase synthesis].

    Science.gov (United States)

    Wang, Ting; Zhu, Yi-Chen; Sun, Zhi-Xuan; Wu, Li-Guang

    2015-02-01

    Photodegradation of pollutions by TiO2 under irradiation of weak UV and visible lights was one of the key points to expand the application of heterogeneous photocatalysis. Based on the adsorption phase synthesis, N doping and co-doping with N and Fe2O3 were employed to prepare TiO2 multi composite photocatalysts. The activity of these photocatalyts was evaluated by photodegradation of methyl-orange illuminated under weak UV and visible lights. Via UV-Vis diffuse reflectance spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy and photoluminescence spectra, the effects on the light absorption and visible response expansion of catalysts caused by different conditions were explored, such as sintering temperature, doping content of N and co-doping. Followed that, the changes in the photocatalytic activities were studied under the irradiation of weak light. The results showed that, N doping could enhance the light absorption of the catalysts, thus significantly enhanced their photocatalytic activity illuminated under UV weak light. All N-doped photocatalysts had a higher activity than the commercial available P25 photocatalyst. The visible response of catalysts was expanded little caused by N doping, thereby most catalysts doped by single N element had no activity illuminated by weak visible light. Only the catalyst doped with 5% of N element showed a weak activity after calcined at 900 degrees C . Due to the synergy effects between N doping and Fe2O3 coupling, co-doping did not only enhance the light absorption of the catalysts, but also significantly expanded the visible response of catalysts. So, co-doped catalysts showed a good catalytic activity when excited by weak visible light.

  7. Preparation of Composite Phase Change Material Based on Sol-Gel Method and Its Temperature-Adjustable Textile

    Institute of Scientific and Technical Information of China (English)

    YI Shi-xiong; MA Xiao-guang; ZHANG Ying; LI Hua

    2009-01-01

    In this study, the sol-gel method was introduced to prepare the composite phase change material (CPCM). The CPCM was added to fabric with coating techniques and the thermal activity of modified fabric was studied. In addition, the thermal property and the microstructure of CPCM were also discussed in detail by means of polarization microscope and differential scanning calorimeter, respectively. According to the analysis of main influencial factors of the property of CPCM, the optimal preparing technique was determined. It was proved that CPCM could exhibit a good thermal property while phase transformation process took place, and a better appearance of the fabric modified with CPCM could be obtained due to the fact that in a warm circumstance, the liquid-state phase change material could be firmly enwrapped and embedded in the three-dimensional network all the time during the phase transformation. Besides, the fabric treated with CPCM had a high phase-transition enthalpy and an appropriate phase-transition temperature. As a result, a desirable temperature-adjustable function appeared.

  8. Phase evolution of(K,Na)NbO3 powder prepared by high temperature mixing under hydrothermal conditions

    Institute of Scientific and Technical Information of China (English)

    Lin Bai; Kongjun Zhu; Jinhao Qiu; Hongli Ji; Likui Su

    2010-01-01

    (Na,K)NbO3(KNN)powders were successfully prepared by high temperature mixing method(HTMM)under hydrothermal conditions to study the effect of reaction time on the formation of KNN for three K+/(K++Na+)ratios of 0.6,0.7 and 0.8.The products were characterized by X-ray diffraction(XRD),scanning electron microscope(SEM),transmission electron microscopy(TEM)and selected area electron diffraction(SAED),to show the change of phase and morphology of the as-prepared particles with the K+/(K++Na+)molar ratio in the solution.Pure Na-rich KNN monoclinic phase and pure K-rich KNN orthorhombic phase could be obtained quickly after mixing the solutions at high temperature when the K+/(K++Na+)molar ratio was either 0.6 or 0.8.When the K+/(K++Na+)molar ratio was 0.7,however,the K-rich KNN orthorhombic phase grain formed first,followed by the Na-rich KNN monoclinic phase grain,with the two phases coexisting in the final product.

  9. Perinatal periods of risk: analytic preparation and phase 1 analytic methods for investigating feto-infant mortality.

    Science.gov (United States)

    Sappenfield, William M; Peck, Magda G; Gilbert, Carol S; Haynatzka, Vera R; Bryant, Thomas

    2010-11-01

    The Perinatal Periods of Risk (PPOR) methods provide the necessary framework and tools for large urban communities to investigate feto-infant mortality problems. Adapted from the Periods of Risk model developed by Dr. Brian McCarthy, the six-stage PPOR approach includes epidemiologic methods to be used in conjunction with community planning processes. Stage 2 of the PPOR approach has three major analytic parts: Analytic Preparation, which involves acquiring, preparing, and assessing vital records files; Phase 1 Analysis, which identifies local opportunity gaps; and Phase 2 Analyses, which investigate the opportunity gaps to determine likely causes of feto-infant mortality and to suggest appropriate actions. This article describes the first two analytic parts of PPOR, including methods, innovative aspects, rationale, limitations, and a community example. In Analytic Preparation, study files are acquired and prepared and data quality is assessed. In Phase 1 Analysis, feto-infant mortality is estimated for four distinct perinatal risk periods defined by both birthweight and age at death. These mutually exclusive risk periods are labeled Maternal Health and Prematurity, Maternal Care, Newborn Care, and Infant Health to suggest primary areas of prevention. Disparities within the study community are identified by comparing geographic areas, subpopulations, and time periods. Excess mortality numbers and rates are estimated by comparing the study population to an optimal reference population. This excess mortality is described as the opportunity gap because it indicates where communities have the potential to make improvement.

  10. Effects of external phase on D-cycloserine loaded W/O nanocapsules prepared by the interfacial polymerization method.

    Science.gov (United States)

    Musumeci, Teresa; Ventura, Cinzia A; Carbone, Claudia; Pignatello, Rosario; Puglisi, Giovanni

    2011-07-01

    Water in oil (W/O) polybutylcyanoacrylate nanocapsules containing D-cycloserine (D-CS) for intranasal delivery were prepared by the interfacial polymerization method. Different oils, as external phase, for the preparation of the initial W/O miniemulsions were used and their effect on mean size and other physico-chemical properties were evaluated by photon correlation spectroscopy (PCS) and scanning electron microscopy (SEM) analysis. Two probes at different hydrophilicity were used to verify the internal aqueous nature of the core. Both miniemulsions and nanocapsules mean size and polydispersity index were influenced by the used external phase. Different entrapment efficiency were obtained for D-cycloserine-loaded nanocapsules correlated to the used oil [ranging from 39 to 51% encapsulation efficiency (E.E.)]. In vitro drug release showed an initial burst effect (ranging from 20 to 40%) followed by a slow release of D-CS for all preparations. This study demonstrated that many relevant physico-chemical and technological properties of polybutylcyanoacrylate nanocapsules prepared by interfacial polymerization of miniemulsions are significantly influenced by the external oil phase used.

  11. Representing Development

    DEFF Research Database (Denmark)

    Representing Development presents the different social representations that have formed the idea of development in Western thinking over the past three centuries. Offering an acute perspective on the current state of developmental science and providing constructive insights into future pathways...... and development, addressing their contemporary enactments and reflecting on future theoretical and empirical directions. The first section of the book provides an historical account of early representations of development that, having come from life science, has shaped the way in which developmental science has...... approached development. Section two focuses upon the contemporary issues of developmental psychology, neuroscience and developmental science at large. The final section offers a series of commentaries pointing to the questions opened by the previous chapters, looking to outline the future lines...

  12. Recombinant Staphylococcal protein A with cysteine residue for preparation of affinity chromatography stationary phase and immunosensor applications

    Directory of Open Access Journals (Sweden)

    Gorbatiuk O. B.

    2015-04-01

    Full Text Available Aim. Engineering of recombinant Staphylococcal protein A with cysteine residue (SPA-Cys for preparation of affinity chromatography stationary phase and formation of bioselective element of immunosensor. Methods. DNA sequences encoding IgG-binding region of SPA, His-tag and cysteine were genetically fused and expressed in E. coli. SPA-Cys was immobilized on maleimide-functionalized silica beads for affinity chromatography stationary phase preparation and on a gold sensor surface as a bioselective element of immunosensor. Results. SPA-Cys was expressed at a high-level in a soluble form. The target protein was purified and showed a high IgG-binding activity. The capacity of the obtained SPA-Cys-based affinity chromatography stationary phase was 10–12 mg of IgG /ml. The purity of eluted IgG was more than 95 % in one-step purification procedure. The developed SPA-Cys-based bioselective element of immunosensor selectively interacted with human IgG and did not interact with the control proteins. Conclusions. The recombinant Staphylococcal protein A with cysteine residue was successfully used for the preparation of affinity chromatography stationary phase and formation of the bioselective element of immunosensor.

  13. Quantitation of antihistamines in pharmaceutical preparations by liquid chromatography with a micellar mobile phase of sodium dodecyl sulfate and pentanol.

    Science.gov (United States)

    Gil-Agustí, M; Monferrer-Pons, L; Esteve-Romero, J; García-Alvarez-Coque, M C

    2001-01-01

    A reversed-phase liquid chromatographic procedure with a micellar mobile phase of sodium dodecyl sulfate (SDS), containing a small amount of pentanol, was developed for the control of 7 antihistamines of diverse action in pharmaceutical preparations (tablets, capsules, powders, solutions, and syrups): azatadine, carbinoxamine, cyclizine, cyproheptadine, diphenhydramine, doxylamine, and tripelennamine. The retention times of the drugs were <9 min with a mobile phase of 0.15M SDS-6% (v/v) pentanol. The recoveries with respect to the declared compositions were in the range of 93-110%, and the intra- and interday repeatabilities and interday reproducibility were <1.2%. The results were similar to those obtained with a conventional 60 + 40 (v/v) methanol-water mixture, with the advantage of reduced toxicity, flammability, environmental impact, and cost of the micellar-pentanol solutions. The lower risk of evaporation of the organic solvent dissolved in the micellar solutions also increased the stability of the mobile phase.

  14. Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase.

    Science.gov (United States)

    Wang, Qing; Long, Yao; Yao, Lin; Xu, Li; Shi, Zhi-Guo; Xu, Lanying

    2016-01-01

    A mixed-mode chromatographic stationary phase, C18-DTT (dithiothreitol) silica (SiO2) was prepared through "thiol-ene" click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen, guanine, tetrandrine and nicotinic acid) in the range of 1.82-3.72% and 0.85-1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids, alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons. It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase.

  15. Controllability study on the preparation of pure phase BiFeO{sub 3} thin films by liquid phase self-assembled method

    Energy Technology Data Exchange (ETDEWEB)

    Ren Xuanru, E-mail: renxuanru1986@163.com [C/C Composites Research Center, State Key Laboratory of Solidification Processing, Northwestern Polytechnical University, Xi' an, Shaanxi 710072 (China); Tan Guoqiang; Miao Hongyan; Li Ziyu [College of Material Science and Engineering, Shaanxi University of Science and Technology, Xi' an, Shaanxi 710021 (China)

    2012-08-01

    Pure phase BiFeO{sub 3} (BFO) thin films were prepared on the ITO/glass substrates covered with functionalized OTS self-assembled monolayers (SAMs) by controllable liquid phase self-assembled method. The hydrophobic surface of OTS-SAMs was changed into hydrophilic surface after UV irradiation, which is helpful to make BFO precursor solutions fully wet the substrate surface. A dense film was formed only on the hydrophilic silnaol group regions, which shows the selectively deposition of BFO precursors. Changing the pH value of BFO precursor solutions will affect the phase purity. The pure phase BFO thin films can be obtained under various pH values, which indicates that the liquid phase self-assembled method is controllable. All pure phase BFO films are dense, smooth, well-grown polycrystalline films, but the size of grains increased gradually along with the increase of pH values. The micropattern of BiFeO{sub 3} film has clear edges. The possible growth mechanism of BFO thin films was discussed.

  16. A Phase Transfer Catalyzed Permanganate Oxidation: Preparation of Vanillin from Isoeugenol Acetate.

    Science.gov (United States)

    Lampman, Gary M.; Sharpe, Steven D.

    1983-01-01

    Background information, laboratory procedures, and results are provided for the preparation of vanillin from isoeugenol acetate. Reaction scheme used to prepare the vanillin and a table indicating the different oxidation experiments carried out on isoeugenol or isoeugenol acetate are also provided. (JN)

  17. Purification of saponins from leaves of Panax notoginseng using preparative two-dimensional reversed-phase liquid chromatography/hydrophilic interaction chromatography.

    Science.gov (United States)

    Guo, Xiujie; Zhang, Xiuli; Feng, Jiatao; Guo, Zhimou; Xiao, Yuansheng; Liang, Xinmiao

    2013-04-01

    Saponins are widely distributed in the plant kingdom and have been shown to be active components of many medicinal herbs. In this study, a two-dimensional purification method based on reversed-phase liquid chromatography coupled with hydrophilic interaction liquid chromatography was successfully applied to purify saponins from leaves of Panax notoginseng. Nine saponin reference standards were used to test the separation modes and columns. The standards could not be resolved using C18 columns owing to their limited polar selectivity. However, they were completely separated on a XAmide column in hydrophilic interaction liquid chromatography mode, including two pairs of standards that were coeluted on a C18 column. The elution order of the standards on the two columns was sufficiently different, with a correlation coefficient between retention times on the C18 and XAmide columns of 0.0126, indicating good column orthogonality. Therefore, the first-dimension preparation was performed on a C18 column, followed by a XAmide column that was used to separate the fractions in the second dimension. Fifty-four fractions were prepared in the first dimension, with 25 fractions rich in saponins. Eight saponins, including two pairs of isomeric saponins and one new saponin, were isolated and identified from three representative fractions. This procedure was shown to be an effective approach for the preparative isolation and purification of saponins from leaves of P. notoginseng. Moreover, this method could possibly be employed in the purification of low-content and novel active saponins from natural products.

  18. Application of spin markers for study of liposome prepared by the modified reverse-phase evaporation method

    OpenAIRE

    Pentak, Danuta; Sułkowski, Wiesław W.; Wolińska, Agnieszka; Maślanka, Sławomir; Bojko, Barbara; Maciążek, Małgorzata; Równicka, Joanna; Sułkowska, Anna

    2008-01-01

    The EPR spectroscopy was used to determine the structure and physicochemical properties of liposomes prepared from L-α-phosphatidylcholine dipalmitoyl (DPPC) by the modified reverse-phase evaporation method (mREV). EPR study was carried out in the temperature range from 297 K to 340 K i.e. below and above the phase transition temperature TC of DPPC. On the basis of EPR spectra of spin marker 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO) incorporated into the liposome, the parameter f was deter...

  19. Direct, preparative enantioselective chromatography of propranolol hydrochloride and thioridazine hydrochloride using carbon dioxide-based mobile phases.

    Science.gov (United States)

    Geiser, F; Schultz, M; Betz, L; Shaimi, M; Lee, J; Champion, W

    1999-12-31

    In this paper, we describe the direct, preparative enantioselective chromatography of racemic (rac)-propranolol hydrochloride (HCI) and rac-thioridazine.HCl using Chiralpak AD chiral stationary phase and mobile phase systems containing carbon dioxide and methanol without the use of basic or acidic additives. Isolated fractions of propranolol.HCl were positively identified by mass spectrometry, Beilstein flame test, melting point, and chemical analysis to be HCI enantiomers of propranolol-HCl salts exhibited characteristic mass spectra peaks at 36 and 38 mass-to-charge ratio in the expected 3:1 isotopic ratio for the solute that were absent in the mass spectra for the free-base forms. To our knowledge, the direct, preparative enantioselective isolation of HCI enantiomeric salts of rac-propranolol and of rac-thioridazine have not been previously demonstrated and published.

  20. Polylactide/acetylated nanocrystalline cellulose composites prepared by a continuous route: A phase interface-property relation study.

    Science.gov (United States)

    Xu, Chunjiang; Chen, Jianxiang; Wu, Defeng; Chen, Yang; Lv, Qiaolian; Wang, Mengqi

    2016-08-01

    A 'continuous route' was developed in this work for the preparation of nanocrystalline cellulose (NCC) filled polylactide (PLA) composites. It combines several separated steps, including extraction of NCC, surface acetylation of NCC, and final composite preparation, into a continuous process, without traditional freeze drying. The obtained PLA composites were then studied in terms of phase interface structure, rheological and mechanical properties. The results reveal that surface acetylation of NCC can improve its affinity to PLA evidently. The thickened interfacial layer makes the system filled with modified NCC show lower percolation threshold than the one filled with pristine NCC; and the former presents a typical strain-scaling stress overshoot behavior in the start-up shear flow because the network structure of modified NCC presents stronger characteristics of self-similarity. The phase interface adhesion also plays an important role in the mechanical behavior of PLA/NCC composites, which is further revealed by the nanomechanical analysis using atom force microscopy.

  1. Parallel preparation of plan-view transmission electron microscopy specimens by vapor-phase etching with integrated etch stops

    Energy Technology Data Exchange (ETDEWEB)

    English, Timothy S., E-mail: englisht@stanford.edu [Department of Mechanical Engineering, Stanford University, Stanford, CA 94305 (United States); Provine, J [Department of Mechanical Engineering, Stanford University, Stanford, CA 94305 (United States); Marshall, Ann F.; Koh, Ai Leen [Stanford Nano Shared Facilities, Stanford University, Stanford, CA 94305 (United States); Kenny, Thomas W. [Department of Mechanical Engineering, Stanford University, Stanford, CA 94305 (United States)

    2016-07-15

    Specimen preparation remains a practical challenge in transmission electron microscopy and frequently limits the quality of structural and chemical characterization data obtained. Prevailing methods for thinning of specimens to electron transparency are serial in nature, time consuming, and prone to producing artifacts and specimen failure. This work presents an alternative method for the preparation of plan-view specimens using isotropic vapor-phase etching with integrated etch stops. An ultrathin amorphous etch-stop layer simultaneously serves as an electron transparent support membrane whose thickness is defined by a controlled growth process such as atomic layer deposition with sub-nanometer precision. This approach eliminates the need for mechanical polishing or ion milling to achieve electron transparency, and reduces the occurrence of preparation induced artifacts. Furthermore, multiple specimens from a plurality of samples can be thinned in parallel due to high selectivity of the vapor-phase etching process. These features enable dramatic reductions in preparation time and cost without sacrificing specimen quality and provide advantages over wet etching techniques. Finally, we demonstrate a platform for high-throughput transmission electron microscopy of plan-view specimens by combining the parallel preparation capabilities of vapor-phase etching with wafer-scale micro- and nanofabrication. - Highlights: • Parallel thinning of plan-view specimens enables high-throughput microscopy studies. • The support membrane thickness is controlled with sub-nanometer precision. • No physical etching (polishing, dimpling, or ion milling) is required. • Large area and uniformly thin specimens are suitable for Cs-corrected HRTEM. • Wafer-scale integration enables custom specimens for in situ experiments.

  2. Preparative crystallization of a single chain antibody using an aqueous two-phase system.

    Science.gov (United States)

    Huettmann, Hauke; Berkemeyer, Matthias; Buchinger, Wolfgang; Jungbauer, Alois

    2014-11-01

    A simultaneous crystallization and aqueous two-phase extraction of a single chain antibody was developed, demonstrating process integration. The process conditions were designed to form an aqueous two-phase system, and to favor crystallization, using sodium sulfate and PEG-2000. At sufficiently high concentrations of PEG, a second phase was generated in which the protein crystallization occurred simultaneously. The single chain antibody crystals were partitioned to the top, polyethylene glycol-rich phase. The crystal nucleation took place in the sodium sulfate-rich phase and at the phase boundary, whereas crystal growth was progressing mainly in the polyethylene glycol-rich phase. The crystals in the polyethylene glycol-rich phase grew to a size of >50 µm. Additionally, polyethylene glycol acted as an anti-solvent, thus, it influenced the crystallization yield. A phase diagram with an undersaturation zone, crystallization area, and amorphous precipitation zone was established. Only small differences in polyethylene glycol concentration caused significant shifts of the crystallization yield. An increase of the polyethylene glycol content from 2% (w/v) to 4% (w/v) increased the yield from approximately 63-87%, respectively. Our results show that crystallization in aqueous two-phase systems is an opportunity to foster process integration.

  3. Superconducting phase prepared from Ta{sub 3}Si under high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Murao, R; Kusaba, K; Fukuoka, K; Sugiyama, K; Syono, Y [IMR, Tohoku University 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); Kikuchi, M [Kansei Fukushi Research Center, Tohoku Fukushi University1-8-1 Kunimi, Aoba-ku, Sendai, Miyagi 981-8522 (Japan); Atou, T [SMC, Materials and Structures Lab. Tokyo Tech. 4259 Nagatsuta-cho Midori-ku, Yokohama, Kanagawa 226-8503 (Japan); Kikegawa, T, E-mail: r_murao@imr.tohoku.ac.j [IMSS, KEK, Oho 1-1, Tsukuba, Ibaraki 305-0801 (Japan)

    2010-03-01

    High-pressure behaviour of Ta{sub 3}Si intermetallic compound was investigated by shock compression and static compression methods. Superconducting phase with T{sub C} = 9.3 K was found in the sample shocked to 50-61 GPa, however most of the shock recovered sample indicated the starting stable phase with the Ti{sub 3}P-type structure. The new superconducting phase was not obtained from static compression up to 15 GPa and 800 {sup 0}C. Bulk modulus of Ta{sub 3}Si with the Ti{sub 3}P-type structure was determined to be K{sub 0} = 246(4) GPa. The present results suggest that a rapid phase transformation occurred during shock compression, but most of the high-pressure phase was reverted to the stable phase in the decompression process.

  4. Preparation of high-pressure phase boron nitride films by physical vapor deposition

    CERN Document Server

    Zhu, P W; Zhao, Y N; Li, D M; Liu, H W; Zou Guang Tian

    2002-01-01

    The high-pressure phases boron nitride films together with cubic, wurtzic, and explosive high-pressure phases, were successfully deposited on the metal alloy substrates by tuned substrate radio frequency magnetron sputtering. The percentage of cubic boron nitride phase in the film was about 50% as calculated by Fourier transform infrared measurements. Infrared peak position of cubic boron nitride at 1006.3 cm sup - sup 1 , which is close to the stressless state, indicates that the film has very low internal stress. Transition electron microscope micrograph shows that pure cubic boron nitride phase exits on the surface of the film. The growth mechanism of the BN films was also discussed.

  5. Study on preparation and thermal properties of sodium nitrate/silica composite as shape-stabilized phase change material

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Qiang [State Key Lab of Chemical Engineering, Department of Chemical Engineering Tsinghua University, Beijing 100084 (China); Postdoctoral Work Station, Shenhua Group Corporation Limited, Beijing 100011 (China); Wang, Tao, E-mail: taowang@tsinghua.edu.cn [State Key Lab of Chemical Engineering, Department of Chemical Engineering Tsinghua University, Beijing 100084 (China)

    2015-08-10

    Highlights: • The NaNO{sub 3}/SiO{sub 2} composite was prepared as shape-stabilized PCM by sol–gel process. • The composite had good thermal energy storage and release ability. • The latent heat was increased with the increase of the roasting temperature. - Abstract: A sodium nitrate (NaNO{sub 3})/silica (SiO{sub 2}) composite was prepared as a shape-stabilized phase change material by a sol–gel procedure. In this composite, NaNO{sub 3} acted as the phase change material and SiO{sub 2} was used as the supporting material. The maximal weight percentage of NaNO{sub 3} in the composite was determined to be 60 wt.%. The chemical composition, morphology, structure and thermal properties were investigated by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), thermal gravimetric analysis (TGA), differential scanning calorimeter (DSC) and Laser thermal conductivity meter. The DSC results indicated that the enthalpies of melting and freezing of the NaNO{sub 3}/SiO{sub 2} (60 wt.% NaNO{sub 3}) composite were 108 kJ/kg and 110 kJ/kg, and the corresponding temperatures of the phase transition were 302 °C and 300 °C, respectively. In the temperature range of lower than 500 °C the phase change enthalpy of the composite was increased with the increase of the roasting temperature.

  6. Preparation and Characterization of Silicone Liquid Core/Polymer Shell Microcapsules via Internal Phase Separation

    DEFF Research Database (Denmark)

    Gonzalez, Lidia; Kostrzewska, Malgorzata; Ma, Baoguang

    2014-01-01

    Microcapsules with a silicone liquid core surrounded by a polymeric shell were synthesisedthrough the controlled phase separation. The dispersed silicone phase consisted of the shellpolymer PMMA, a good solvent for the PMMA (dichloromethane, DCM) and a poor solvent(methylhydrosiloxane dimethylsil...

  7. Main corrective measures in an early phase of nuclear power plants’ preparation for safe long term operation

    Energy Technology Data Exchange (ETDEWEB)

    Krivanek, Robert, E-mail: r.krivanek@iaea.org [International Atomic Energy Agency (IAEA), Department of Nuclear Safety and Security, Operational Safety Section, Vienna 1400 (Austria); Fiedler, Jan, E-mail: fiedler@fme.vutbr.cz [University of Technology Brno, Faculty of Mechanical Engineering, Energy Institute, Technická 2896/2, 616 69 Brno (Czech Republic)

    2017-05-15

    Highlights: • Results of SALTO missions provide the most important issues for safe long term operation (LTO) of nuclear power plants. • The most important technical corrective measures in an early phase of preparation for safe LTO are described. • Their satisfactory resolution creates a basis for further activities to demonstrate preparedness for safe LTO. - Abstract: This paper presents the analysis of main technical deficiencies of nuclear power plants (NPPs) in preparedness for safe long term operation (LTO) and the main corrective measures in an early phase of preparation for safe LTO of NPPs. It focuses on technical aspects connected with management of physical ageing of NPP structures, systems and components (SSCs). It uses as a basis results of IAEA SALTO missions performed between 2005 and 2016 (see also paper NED8805 in Nuclear Engineering and Design in May 2016) and the personal experiences of the authors with preparation of NPPs for safe LTO. This paper does not discuss other important aspects of safe LTO of NPPs, e.g. national nuclear energy policies, compliance of NPPs with the latest international requirements on design, obsolescence, environmental impact and economic aspects of LTO. Chapter 1 provides a brief introduction of the current status of the NPP’ fleet in connection with LTO. Chapter 2 provides an overview of SALTO peer review service results with a focus on deficiencies related to physical ageing of safety SSCs and a demonstration that SSCs will perform their safety function during the intended period of LTO. Chapter 3 discusses the main corrective measures which NPPs typically face during the preparation for demonstration of safe LTO. Chapter 4 summarizes the current status of the NPP’ fleet in connection with LTO and outlines further steps needed in preparation for safe LTO.

  8. Purification of amide alkaloids from Piper longum L. using preparative two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography.

    Science.gov (United States)

    Li, Kuiyong; Zhu, Wenya; Fu, Qing; Ke, Yanxiong; Jin, Yu; Liang, Xinmiao

    2013-06-07

    A comprehensive off-line two-dimensional liquid chromatography (2D-LC) method coupling normal phase liquid chromatography (NPLC) and reversed phase liquid chromatography (RPLC) was developed for separation and purification of amide alkaloids from Piper longum L. In the first dimension, the crude alkaloid fractions were separated in NPLC mode and 20 fractions were collected. Then fractions 5-20 were selected for further purification in RPLC mode in the second dimension. The purities of RPLC fractions with similar structures were all identified accurately by ultra performance liquid chromatography (UPLC). In total, 28 compounds with high purity were obtained and their structures were comprehensively characterized by electrospray ionization-mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR) spectroscopy. The results demonstrate that this 2D NPLC × RPLC method with good orthogonality (58.3%) was effective for the preparative separation and purification of amide alkaloids from Piper longum L.

  9. On-line comprehensive two-dimensional normal-phase liquid chromatography×reversed-phase liquid chromatography for preparative isolation of toad venom.

    Science.gov (United States)

    Li, Jia-Fu; Fang, Hua; Yan, Xia; Chang, Fang-Rong; Wu, Zhen; Wu, Yun-Long; Qiu, Ying-Kun

    2016-07-22

    An on-line comprehensive preparative two-dimensional normal-phase liquid chromatography×reversed-phase liquid chromatography (2D NPLC×RPLC) system was constructed with a newly developed vacuum evaporation assisted adsorption (VEAA) interface, allowing fast removal of NPLC solvent in the vacuum condition and successfully solving the solvent incompatibility problem between NPLC and RPLC. The system achieved on-line solvent exchange within the two dimensions and its performance was illustrated by gram-scale isolation of crude extract from the venom of Bufo bufo gargarizans. Within separation time of ∼20h, 19 compounds were obtained with high purity in a single run. With the VEAA interface, the 2D system exhibited apparent advantages in separation efficiency and automation compared with conventional methods, indicating its promising application in the routine separation process for complicated natural products.

  10. Western Kentucky University's Teacher Preparation Evaluation Model Phase I, Cycle I. Annual Report.

    Science.gov (United States)

    Adams, Ronald D.

    A teacher preparation evaluation model was developed at Western Kentucky University. A total of 18 secondary and 20 elementary student teachers participated in the study. Instrumentation and records used for data collection consisted of five general types: a questionnaire, a personality scale, rating scales, direct classroom observational systems,…

  11. Preparation and evaluation of monolithic molecularly imprinted stationary phase for S-naproxen

    Institute of Scientific and Technical Information of China (English)

    De-Miao Chen; Qiang Fu; Wei Du; Si-Juan Sun; Ping Huang; Chun Chang

    2011-01-01

    An S-naproxen(S-NAP)molecularly imprinted monolithic stationary phase(MIMSP)with specific recognition for S-NAP and naproxen(NAP)was prepared by in situ technique,utilizing 4-vinylpridine(4-VP)as a function monomer,ethylene glycol dimethacrylate(EDMA)as a

  12. Preparation of titania particles utilizing the insoluble phase interface in a microchannel reactor.

    Science.gov (United States)

    Wang, Hongzhi; Nakamura, Hiroyuki; Uehara, Masato; Miyazaki, Masaya; Maeda, Hideaki

    2002-07-21

    A stable interface between two insoluble currents in a microchannel reactor has been obtained by selecting the solvents and adjusting the flow rate; titania particles with a size of less than 10 nm could be prepared continuously on this interface; this new method shows great advantage for the control and measurement of particle sizes.

  13. Lipid mixtures prepared with well-defined synthetic ceramides closely mimic the unique stratum corneum lipid phase behavior.

    Science.gov (United States)

    de Jager, Miranda W; Gooris, Gert S; Ponec, Maria; Bouwstra, Joke A

    2005-12-01

    Lipid lamellae present in the outermost layer of the skin, the stratum corneum, form the main barrier for the diffusion of molecules through the skin. The presence of a unique 13 nm lamellar phase and its high crystallinity are characteristic for the stratum corneum lipid phase behavior. In the present study, small-angle and wide-angle X-ray diffraction were used to examine the organization in lipid mixtures prepared with a unique set of well-defined synthetic ceramides, varying from each other in head group architecture and acyl chain length. The results show that equimolar mixtures of cholesterol, free fatty acids, and synthetic ceramides (resembling the composition of pig ceramides) closely resemble the lamellar and lateral stratum corneum lipid organization, both at room and higher temperatures. Exclusion of several ceramide classes from the mixture does not affect the lipid organization. However, complete substitution of ceramide 1 (acylceramide with a sphingosine base) with ceramide 9 (acylceramide with a phytosphingosine base) reduces the formation of the long periodicity lamellar phase. This indicates that the head group architecture of acylceramides affects the lipid organization. In conclusion, lipid mixtures prepared with well-defined synthetic ceramides offer an attractive tool with which to unravel the importance of the molecular structure of individual ceramides for proper lipid organization.

  14. Preparation, characterization and thermal properties of binary nitrate salts/expanded graphite as composite phase change material

    Energy Technology Data Exchange (ETDEWEB)

    Xiao, Junbing [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China); Huang, Jin, E-mail: huangjiner@126.com [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China); Zhu, Panpan; Wang, Changhong [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China); Li, Xinxi [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China); Center for Nanochemistry, Beijing National Laboratory for Molecular Sciences, State Key Laboratory for Structural Chemistry of Unstable and Stable Species, College of Chemistry and Molecular Engineering, Peking University, Beijing (China)

    2014-07-01

    Highlights: • The expanded graphite enhanced thermal conductivity coefficient greatly. • The aqueous solution method adopting ultrasonic was utilized to disperse EG. • The combination of composite was physical without chemical reaction. • The reduction on total latent heat was slight after the adding EG. - Abstract: The binary nitrate salts/expanded graphite (EG) composite phase change material (PCM) were prepared via adding different mass rate of EG to binary nitrate salts consisting of NaNO{sub 3} and KNO{sub 3} (6:4) by aqueous solution method adopting ultrasonic. The morphology and chemical composition of EG and the composite PCM were characterized and investigated by X-ray diffraction (XRD), scan electron microscope (SEM), energy dispersive spectrometer (EDS), transmission electron microscope (TEM), respectively. Laser thermal conductivity instrument and differential scanning calorimeter (DSC) were employed to measure thermo physical properties. Drawing the conclusion from investigation, that EG had enhanced thermal conductivity coefficient which largely increased to 4.884 W/(m K) and reduced total latent heat by mostly 11.0%. The morphology and phase structure results indicated that EG were well dispersed into and physically combined with molten salts. In general, the prepared composite PCM could be a suitable phase change material for thermal energy storage.

  15. Preparation and Characterization of Hydrophilically Modified PVDF Membranes by a Novel Nonsolvent Thermally Induced Phase Separation Method

    Directory of Open Access Journals (Sweden)

    Ningen Hu

    2016-11-01

    Full Text Available In this study, a nonsolvent thermally-induced phase separation (NTIPS method was first proposed to fabricate hydrophilically-modified poly(vinylidene fluoride (PVDF membranes to overcome the drawbacks of conventional thermally-induced phase separation (TIPS and nonsolvent-induced phase separation (NIPS methods. Hydrophilically-modified PVDF membranes were successfully prepared by blending in hydrophilic polymer polyvinyl alcohol (PVA at 140 °C. A series of PVDF/PVA blend membranes was prepared at different total polymer concentrations and blend ratios. The morphological analysis via SEM indicated that the formation mechanism of these hydrophilically-modified membranes was a combined NIPS and TIPS process. As the total polymer concentration increased, the tensile strength of the membranes increased; meanwhile, the membrane pore size, porosity and water flux decreased. With the PVDF/PVA blend ratio increased from 10:0 to 8:2, the membrane pore size and water flux increased. The dynamic water contact angle of these membranes showed that the hydrophilic properties of PVDF/PVA blend membranes were prominently improved. The higher hydrophilicity of the membranes resulted in reduced membrane resistance and, hence, higher permeability. The total resistance Rt of the modified PVDF membranes decreased significantly as the hydrophilicity increased. The irreversible fouling related to pore blocking and adsorption fouling onto the membrane surface was minimal, indicating good antifouling properties.

  16. Preparation of Paraffin/γ-Al2O3Composites as Phase Change Energy Storage Materials%Preparation of Paraffin/γ-Al2O3 Composites as Phase Change Energy Storage Materials

    Institute of Scientific and Technical Information of China (English)

    ZHAO Liang; MARuiying; MENG Xianglan; WANG Gang; FANG Xiangchen

    2011-01-01

    Paraffin/γ-Al2O3 composites as phase change energy storage materials were prepared by absorbingparaffin in porous network of γ-Al2O3.In the composite materials,paraffin was used as a phase change material(PCM) for thermal energy storage,and γ-Al2O3 acted as supporting materials.Characterizations were conducted to evaluate the energy storage performance of the composites,and differential scanning calorimeter results showed that the PCM-3 composite has melting latent heat of 112.9 kJ/kg with a melting temperature of 62.9 ℃.Due to strong capillary force and surface tension between paraffin and γ-Al2O3,the leakage of melted paraffin from the composites can be effectively prevented.Therefore,the paraffin/γ-Al2O3 composites have a good thermal stability and can be used repeatedly.

  17. Structural and phase characterization of bioceramics prepared from tetracalcium phosphate-monetite cement and in vitro osteoblast response.

    Science.gov (United States)

    Stulajterova, Radoslava; Medvecky, Lubomir; Giretova, Maria; Sopcak, Tibor

    2015-05-01

    Biphasic porous calcium phosphate ceramics was prepared by sintering of transformed tetracalcium phosphate-monetite cement. After annealing hydroxyapatite, β- or α-TCP were found as main phases in ceramic substrates and a highly microporous microstructure of cement ceramics was created without an addition of porosifier. The origin microstructure features characteristic by the presence of hollow particle agglomerates in cement were preserved in microstructure of cement ceramics after annealing but the hydroxyapatite particles rose in size up to 2 µm and obtained a more regular shape. A small decrease in compressive strength was demonstrated in ceramics sintered up to 1150 °C and enhanced osteoblast proliferation was revealed on cement ceramic substrates in comparison with cement sample and conventional ceramics. The ALP activity of osteoblasts decreased with rise in sintering temperature. The prepared cement microporous ceramics could be utilized as carrier for antibiotics, drugs, growth factors, enzymes or other substances stimulating healing process.

  18. Preparation and evaluation of novel chiral stationary phases based on quinine derivatives comprising crown ether moieties.

    Science.gov (United States)

    Wang, Dongqiang; Zhao, Jianchao; Wu, Haixia; Wu, Haibo; Cai, Jianfeng; Ke, Yanxiong; Liang, Xinmiao

    2015-01-01

    The C9-position of quinine was modified by meta- or para-substituted benzo-18-crown-6, and immobilized on 3-mercaptopropyl-modified silica gel through the radical thiol-ene addition reaction. These two chiral stationary phases were evaluated by chiral acids, amino acids, and chiral primary amines. The crown ether moiety on the quinine anion exchanger provided a ligand-exchange site for primary amino groups, which played an important role in the retention and enantioselectivity for chiral compounds containing primary amine groups. These two stationary phases showed good selectivity for some amino acids. The complex interaction between crown ether and protonated primary amino group was investigated by the addition of inorganic salts such as LiCl, NH4Cl, NaCl, and KCl to the mobile phase. The resolution results showed that the simultaneous interactions between two function moieties (quinine and crown ether) and amino acids were important for the chiral separation.

  19. The preparation of the Ti-Al alloys based on intermetallic phases

    Science.gov (United States)

    Kosova, N.; Sachkov, V.; Kurzina, I.; Pichugina, A.; Vladimirov, A.; Kazantseva, L.; Sachkova, A.

    2016-01-01

    This article deals with a method of obtaining materials in the Ti-Al system. Research was carried out in accordance with the phase diagram of the system state. It was established, that both single-phase and multiphase systems, containing finely dispersed intermetallic compositions of phases Ti3Al, TiAl and TiAl3, are formed. Additionally, it was found that the pure finely dispersed (coherent-scattering region (CSR) up to 100 nm) intermetallic compound TiAl3 is formed at molar ratio of Ti:Al = 1:3. Experimentally proved the possibility of produce the complex composition of alloys and intermetallic compounds and products based on them.

  20. Preparation of {sup 183,184}Re samples for modelling a rapid gas phase chemistry of Nielsbohrium (Ns), element 107

    Energy Technology Data Exchange (ETDEWEB)

    Eichler, R.; Gaeggeler, H.W.; Eichler, B.; Tuerler, A. [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-09-01

    Chemical gas phase reactions of the heavier group 7 elements in the system O{sub 2}/H{sub 2}O are presumably best suited for a separation of Nielsbohrium from the lighter transactinides. We expect a higher reaction velocity using the more reactive gas system O{sub 3}/H{sub 2}O{sub 2}. For the experimental verification of this idea we prepared {sup 183}Re/{sup 184}Re samples for thermochromatography experiments with both gas systems. (author) 8 refs.

  1. Polymer composites and porous materials prepared by thermally induced phase separation and polymer-metal hybrid methods

    Science.gov (United States)

    Yoon, Joonsung

    The primary objective of this research is to investigate the morphological and mechanical properties of composite materials and porous materials prepared by thermally induced phase separation. High melting crystallizable diluents were mixed with polymers so that the phase separation would be induced by the solidification of the diluents upon cooling. Theoretical phase diagrams were calculated using Flory-Huggins solution thermodynamics which show good agreement with the experimental results. Porous materials were prepared by the extraction of the crystallized diluents after cooling the mixtures (hexamethylbenzene/polyethylene and pyrene/polyethylene). Anisotropic structures show strong dependence on the identity of the diluents and the composition of the mixtures. Anisotropic crystal growth of the diluents was studied in terms of thermodynamics and kinetics using DSC, optical microscopy and SEM. Microstructures of the porous materials were explained in terms of supercooling and dendritic solidification. Dual functionality of the crystallizable diluents for composite materials was evaluated using isotactic polypropylene (iPP) and compatible diluents that crystallize upon cooling. The selected diluents form homogeneous mixtures with iPP at high temperature and lower the viscosity (improved processability), which undergo phase separation upon cooling to form solid particles that function as a toughening agent at room temperature. Tensile properties and morphology of the composites showed that organic crystalline particles have the similar effect as rigid particles to increase toughness; de-wetting between the particle and iPP matrix occurs at the early stage of deformation, followed by unhindered plastic flow that consumes significant amount of fracture energy. The effect of the diluents, however, strongly depends on the identity of the diluents that interact with the iPP during solidification step, which was demonstrated by comparing tetrabromobisphenol-A and

  2. Geopolymers prepared from DC plasma treated air pollution control (APC) residues glass: properties and characterisation of the binder phase.

    Science.gov (United States)

    Kourti, Ioanna; Devaraj, Amutha Rani; Bustos, Ana Guerrero; Deegan, David; Boccaccini, Aldo R; Cheeseman, Christopher R

    2011-11-30

    Air pollution control (APC) residues have been blended with glass-forming additives and treated using DC plasma technology to produce a high calcium aluminosilicate glass (APC glass). This has been used to form geopolymer-glass composites that exhibit high strength and density, low porosity, low water absorption, low leaching and high acid resistance. The composites have a microstructure consisting of un-reacted residual APC glass particles imbedded in a complex geopolymer and C-S-H gel binder phase, and behave as particle reinforced composites. The work demonstrates that materials prepared from DC plasma treated APC residues have potential to be used to form high quality pre-cast products.

  3. Synthesis of oligodeoxyribonucleotides by solid phase phosphotriester method on a reduced scale; preparation of oligonucleotides for improved promoter sequence.

    Science.gov (United States)

    Naruto, M

    1982-01-01

    A small reaction vessel, composed of a balled sintered glass filter and a test tube with a stopcock, was designed for the solid phase phosphotriester synthesis of oligodeoxyribonucleotide. Operation of small scale synthesis (nucleoside on resin: 3-6 mumol, activated diester of dimer: 20-30 mumol) was performed under the atmosphere of argon. The yield of each coupling reaction was 60-100%. Twelve short oligonucleotides (6-16mer) were obtained in 19-78% overall yield by this method. These oligomers were prepared as a part of the control region of gene to increase the translation efficiency.

  4. Preparative isolation of Heteroclitin D from Kadsurae Caulis using normal-phase flash chromatography

    Institute of Scientific and Technical Information of China (English)

    Xiao-Xue Yu; Qian-Wen Wang; Xin-Jun Xu; Wei-Jian Lv; Ming-Qian Zhao; Zhi-Kun Liang

    2013-01-01

    Heteroclitin D (H.D) was successfully isolated from Kadsurae Caulis by using flash chromatography and recrystallized by methanol, 10.2 mg of H.D was obtained from 4.86 g of crude extract, and the purity determined by HPLC was 99.4%. The structure was identified by UV, IR, MS, and NMR analysis. The fast, simple and efficient method can be applied to the preparation of reference substance of H. D.

  5. Phase Development and Crystallization Kinetics of NiTi Prepared by Mechanical Alloying

    Institute of Scientific and Technical Information of China (English)

    Xunyong JIANG; Xueping GAO; Deying SONG

    2003-01-01

    NiTi alloy is produced by mechanical alloying(MA). It becomes amorphous after milling for enough time, such as 100 h in this paper. DSC measurement shows that the crystallization temperature is 676 K for the amorphous powder. Activation energy of crystallization is 199.98 kJ/mol for MA powder, which is lower than that of amorphous prepared by magnetron sputtering.Avrami parameter of crystallization is 1.07.

  6. Photocatalytic Studies of Anatase and Rutile phase TiO2 Nanocrystals Prepared via Solvothermal method

    Directory of Open Access Journals (Sweden)

    S.Perumal

    2015-08-01

    Full Text Available Nanocrystals of TiO2 photocatalyst have been synthesized by solvothermal method. The photocatalysts were characterized by XRD, UV–Vis spectroscopy and photocatalytic study. The analysis from X-ray diffraction revealed that the annealed product at 1000˚C shows crystal phase of rutile and all others are in anatase phase. FTIR spectra show the vibration of Ti-O bands around 650 cm-1 . UV-Vis spectra indicated the band gap value of annealed samples.

  7. Preparation of Surface Organometallic Catalysts by Gas-Phase Ligand Stripping and Reactive Landing of Mass-Selected Ions

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, Grant E.; Laskin, Julia

    2010-12-27

    Organometallic complexes immobilized on surfaces combine the high selectivity of homogeneous catalysts with the ease of separation of catalyst from products of heterogeneous materials. Here we report a novel approach for the highly controlled preparation of surface organometallic catalysts by gas-phase ligand stripping combined with reactive landing of mass-selected ions onto self assembled monolayer surfaces. Collision induced dissociation is used to generate highly reactive undercoordinated metal complexes in the gas-phase for subsequent surface immobilization. Complexes with an open coordination shell around the metal center are demonstrated to show enhanced activity towards reactive landing in comparison to fully ligated species. In situ TOF-SIMS analysis indicates that the immobilized complexes exhibit behaviour consistent with catalytic activity when exposed to gaseous reagents.

  8. Preparation and characterization of form-stable paraffin/polycaprolactone composites as phase change materials for thermal energy storage

    Directory of Open Access Journals (Sweden)

    Aludin M.S.

    2017-01-01

    Full Text Available Paraffin is Phase Change Materials (PCM that possesses desirable properties such as high thermal energy storage and thermal stability to make it suitable for thermal energy storage applications. However, paraffin has been reported to leak out during the melting process. In this study, composites were prepared by dissolving paraffin and polycaprolactone (PCL at varied mass percent compositions in chloroform and then purified through precipitation techniques. The leakage test was conducted by placing the composite samples on a set of four-layer filter papers and left in a furnace at 90°C for 1 hour. By incorporating PCL into paraffin phase, the leakage mass percentage was drastically reduced. The PCL polymer matrix in the composites may have trapped the paraffin molecules during melting process thus prevent it from leaking.

  9. Graphene-Based Materials as Solid Phase Extraction Sorbent for Trace Metal Ions, Organic Compounds, and Biological Sample Preparation.

    Science.gov (United States)

    Ibrahim, Wan Aini Wan; Nodeh, Hamid Rashidi; Sanagi, Mohd Marsin

    2016-07-03

    Graphene is a new carbon-based material that is of interest in separation science. Graphene has extraordinary properties including nano size, high surface area, thermal and chemical stability, and excellent adsorption affinity to pollutants. Its adsorption mechanisms are through non-covalent interactions (π-π stacking, electrostatic interactions, and H-bonding) for organic compounds and covalent interactions for metal ions. These properties have led to graphene-based material becoming a desirable adsorbent in a popular sample preparation technique known as solid phase extraction (SPE). Numerous studies have been published on graphene applications in recent years, but few review papers have focused on its applications in analytical chemistry. This article focuses on recent preconcentration of trace elements, organic compounds, and biological species using SPE-based graphene, graphene oxide, and their modified forms. Solid phase microextraction and micro SPE (µSPE) methods based on graphene are discussed.

  10. Preparation of niobium based oxynitride nanosheets by exfoliation of Ruddlesden-Popper phase precursor

    Science.gov (United States)

    da Silva Maia, Ary; Cheviré, François; Demange, Valérie; Bouquet, Valérie; Pasturel, Mathieu; Députier, Stéphanie; Lebullenger, Ronan; Guilloux-Viry, Marylline; Tessier, Franck

    2016-04-01

    A new oxynitride Ruddlesden-Popper phase K1.6Ca2Nb3O9.4N0.6.1.1H2O was synthesized by the topochemical ammonolysis reaction at 700 °C from the oxide Dion-Jacobson phase KCa2Nb3O10 in the presence of K2CO3. The oxynitride showed good stability with a little loss of nitrogen, even after a few months of exposure to air. Its crystal structure was solved by Rietveld refinement of X-ray powder diffraction data in space group P4/mmm and considering a two-phase mixture, due to the difference in the degree of hydration, with a = 3.894(2) Å and c = 17.90(8) Å for the most hydrated phase and a = 3.927(6) Å and c = 17.09(2) Å for the less one. Optical band gaps were measured by diffuse reflectance in the UV-Visible range indicating a red shift of Eg to the visible region. The oxynitride layered perovskite was then protonated and exfoliated into nanosheets. TEM images and SAED patterns of the nanosheets proved that exfoliation was successful, showing lattice parameters quite compatible with the Rietveld refinement.

  11. New method for the preparation of solid-phase bound isocyanocarboxylic acids and Ugi reactions therewith

    NARCIS (Netherlands)

    Henkel, Bernd; Sax, Michael; Dömling, Alexander

    2003-01-01

    A novel method of synthesizing solid-phase bound isocyanocarboxylic acids is reported. The potassium salts of four different isocyanocarboxylic acids are coupled onto a brominated resin in DMF in good yields. 32 Ugi reactions were performed using these resins and 24 products were obtained in good to

  12. Integrated Automation of High-Throughput Screening and Reverse Phase Protein Array Sample Preparation

    DEFF Research Database (Denmark)

    Pedersen, Marlene Lemvig; Block, Ines; List, Markus

    multiplexing readouts, but this has a natural limitation. High-content screening via image acquisition and analysis allows multiplexing of few parameters, but is connected to substantial time consumption and complex logistics. We report on integration of Reverse Phase Protein Arrays (RPPA)-based readouts...

  13. Simplifying sample preparation using fabric phase sorptive extraction technique for the determination of benzodiazepines in blood serum by high-performance liquid chromatography.

    Science.gov (United States)

    Samanidou, Victoria; Kaltzi, Ioanna; Kabir, Abuzar; Furton, Kenneth G

    2016-06-01

    Fabric phase sorptive extraction (FPSE), a recently introduced novel sample preparation technology, has been evaluated for the extraction of benzodiazepines from human blood serum. FPSE utilizes a flexible fabric surface as the substrate platform for creating sol-gel hybrid organic-inorganic sorbent coatings. FPSE media can be introduced directly into the sample containing the target analyte(s), requiring no need for prior sample pretreatment or clean-up. Benzodiazepines were selected as model analytes because they represent one of the most widely used therapeutic drugs in psychiatry and are also amongst the most frequently encountered drugs in forensic toxicology. The chromatographic separation of target analytes was performed on a LiChroCART-LiChrospher®100 RP-18e (5 µm, 250 × 4 mm) analytical column, operated at room temperature. Ternary gradient elution was applied with a mobile phase that consisted of acetonitrile, methanol and ammonium acetate (0.05 M), which was delivered at a flow rate of 1.0 mL/min. Diode array detection was performed with monitoring at 240 nm. FPSE was performed using cellulose fabric extraction media coated with sol-gel poly(ethylene glycol) (sol-gel PEG). Absolute recovery values in the equilibrium state for the examined benzodiazepines were found to be 27% for bromazepam, 63% for lorazepam, 42 % for diazepam and 39% for alprazolam. Copyright © 2015 John Wiley & Sons, Ltd.

  14. Preparation and evaluation of surface-bonded tricationic ionic liquid silica as stationary phases for high-performance liquid chromatography.

    Science.gov (United States)

    Qiao, Lizhen; Shi, Xianzhe; Lu, Xin; Xu, Guowang

    2015-05-29

    Two tricationic ionic liquids were prepared and then bonded onto the surface of supporting silica materials through "thiol-ene" click chemistry as new stationary phases for high-performance liquid chromatography. The obtained columns of tricationic ionic liquids were evaluated respectively in the reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode, and possess ideal column efficiency of 80,000 plates/m in the RPLC mode with naphthalene as the test solute. The tricationic ionic liquid stationary phases exhibit good hydrophobic and shape selectivity to hydrophobic compounds, and RPLC retention behavior with multiple interactions. In the HILIC mode, the retention and selectivity were evaluated through the efficient separation of nucleosides and bases as well as flavonoids, and the typical HILIC retention behavior was demonstrated by investigating retention changes of hydrophilic solutes with water volume fraction in mobile phase. The results show that the tricationic ionic liquid columns possess great prospect for applications in analysis of hydrophobic and hydrophilic samples.

  15. Preparation, characterization, and thermal properties of the microencapsulation of a hydrated salt as phase change energy storage materials

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Jin, E-mail: huangjiner@126.com [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China); Wang, Tingyu; Zhu, Panpan; Xiao, Junbin [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China)

    2013-04-10

    Highlights: ► Phase change point and fusion heat of samples are about 51 °Cand 150 J/g respectively. ► DSC results indicated the core material is not Na{sub 2}HPO{sub 4}·12H{sub 2}O but Na{sub 2}HPO{sub 4}·7H{sub 2}O. ► Encapsulation takes a significant role in reducing subcooling degree. - Abstract: Microcapsules loaded by disodium hydrogen phosphate heptahydrate (Na{sub 2}HPO{sub 4}·7H{sub 2}O) were prepared by means of the suspension copolymerization-solvent volatile method, with modified polymethylmethacrylate (PMMA) as coating polymer under the conditions of various organic solvents. The formation of the microencapsulated phase change materials (MEPCMs)-PMMA/Na{sub 2}HPO{sub 4}·7H{sub 2}O was investigated and analyzed. The morphology of the resultant materials was characterized by using scanning electron microscope (SEM) and phase contrast microscope. Its final composition was confirmed by the Fourier transformation infrared (FT-IR). Thermo gravimetric analyzer (TGA) and differential scanning calorimetry (DSC) were adopted to reveal its thermal stability and thermal properties. Results indicated that the materials owned improved subcooling degree and good thermal properties, enabling the materials to be one promising phase change materials for thermal energy storage.

  16. Preparation and mechanical properties of liquid-phase sinterd silicon carbide; Herstellung und mechanische Eigenschaften von fluessigphasengesintertem Siliziumkarbid

    Energy Technology Data Exchange (ETDEWEB)

    Wiedmann, I.

    1998-12-01

    Liquid-phase sintered silicon carbide ceramics, LPS-SiC, were prepared, and the influence of structure and chemical secondary phase composition on the mechanical properties was investigated in order to identify LPS-SiC materials which can be produced reproducibly and with low loss of mass by simple techniques, i.e. without powder bed or encapsulation. Their profile of characteristics should be superior to conventional solid-phase sintered SiC and should be comparable with liquid-phase sintered silicon nitride ceramics. [Deutsch] In der vorliegenden Arbeit wurden fluessigphasengesinterte Siliziumkarbid-Keramiken, LPS-SiC, hergestellt und der Einfluss der Gefuegeausbildung und der chemischen Sekundaerphasenzusammensetzung auf die mechanischen Eigenschaften untersucht. Ziel war es, LPS-SiC-Materialien zu identifizieren, die ohne besonderen Vorkehrungen wie Pulverbett oder Einkapselung reproduzierbar und mit geringem Masseverlust hergestellt werden koennen. Das Eigenschaftsprofil sollte deutlich ueber dem von konventionell festphasengesintertem SiC liegen und vergleichbar zu fluessigphasengesinterten Siliziumnitrid-Keramiken sein. (orig.)

  17. Perpentylated (2, 3, 6-Tri-O-pentyl)-β-cyclodextrin Used as Capillary Gas Chromatographic Stationary Phase Prepared by Sol-gel Technology

    Institute of Scientific and Technical Information of China (English)

    Min Min LIANG; Mei Ling QI; Yu LENG; Ruo Nong FU

    2005-01-01

    Capillary column preparation using perpentylated (2,3,6-tri-O-pentyl)-β-cyclodextrin as stationary phase by sol-gel technology with simplicity and rapidity is described. Multiple preparation steps in conventional column technology were avoided. The prepared columns exhibit satisfactory chromatographic performances and pronounced selectivity for a wide range of test solutes, and have been successfully used for the separation of nitrotoluene, dimethoxybenzene,alcohols, alkanes, dimethylphenol and cresol isomers.

  18. Effect of preparation conditions on the nanostructure of hydroxyapatite and brushite phases

    Directory of Open Access Journals (Sweden)

    S. F. Mansour

    2015-11-01

    Full Text Available Abstract Hydroxyapatite (HAP and dicalcium phosphate dihydrate (brushite nanoparticles were prepared by co-precipitation method. The obtained products were characterized by X-ray powder diffraction (XRD, Fourier transformation infra-red spectroscopy (FTIR and thermo-gravimetric analysis (TGA. Scanning electron microscopy (SEM and transmission electron microscope (TEM were used to investigate the morphology of the powdered samples as well as their microstructure, respectively. Brushite samples were obtained in a spherical shape, while hydroxyapatite was formed in a needle and rice shape depending on the pH value.

  19. Atomic pairwise distribution function analysis of the amorphous phase prepared by different manufacturing routes

    DEFF Research Database (Denmark)

    Boetker, Johan P.; Koradia, Vishal; Rades, Thomas

    2012-01-01

    was subjected to quench cooling thereby creating an amorphous form of the drug from both starting materials. The milled and quench cooled samples were, together with the crystalline starting materials, analyzed with X-ray powder diffraction (XRPD), Raman spectroscopy and atomic pair-wise distribution function...... (PDF) analysis of the XRPD pattern. When compared to XRPD and Raman spectroscopy, the PDF analysis was superior in displaying the difference between the amorphous samples prepared by milling and quench cooling approaches of the two starting materials....

  20. Effect of preparation conditions on the nanostructure of hydroxyapatite and brushite phases

    Science.gov (United States)

    Mansour, S. F.; El-dek, S. I.; Ahmed, M. A.; Abd-Elwahab, S. M.; Ahmed, M. K.

    2016-10-01

    Hydroxyapatite (HAP) and dicalcium phosphate dihydrate (brushite) nanoparticles were prepared by co-precipitation method. The obtained products were characterized by X-ray powder diffraction (XRD), Fourier transformation infra-red spectroscopy (FTIR) and thermo-gravimetric analysis (TGA). Scanning electron microscopy (SEM) and transmission electron microscope (TEM) were used to investigate the morphology of the powdered samples as well as their microstructure, respectively. Brushite samples were obtained in a spherical shape, while hydroxyapatite was formed in a needle and rice shape depending on the pH value.

  1. A solid-phase microextraction fiber with carbon nanoparticles as sorbent material prepared by a simple flame-based preparation process.

    Science.gov (United States)

    Sun, Min; Feng, Juanjuan; Qiu, Huamin; Fan, Lulu; Li, Leilei; Luo, Chuannan

    2013-07-26

    A novel carbon nanoparticles-coated solid-phase microextraction (SPME) fiber was prepared via a simple and low-cost flame-based preparation process, with stainless steel wire as support. Surface characteristic of the fiber was studied with scanning electron microscope. A nano-scaled brushy structure was observed. Coupled to gas chromatography (GC), the fiber was used to extract phthalate esters (PAEs) and polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Analytical performances of the proposed method were investigated under the optimum extraction conditions (extraction temperature, 40°C; content of KCl, 30% (w/v); extraction time, 50min for PAEs and 40min for PAHs) and compared with other reports for the same analytes. Calibration ranges were 0.06-500μgL(-1) for di-n-butyl phthalate (DBP), and 0.1-300μgL(-1) for di-cyclohexyl phthalate (DCHP) and di-(2-ethyl-hexyl) phthalate (DEHP). For the eight PAHs, good linearity was obtained ranging from 0.01 to 150μgL(-1). Limits of detection were 0.005μgL(-1) for three PAEs and 0.001-0.003μgL(-1) for eight PAHs. The fiber exhibited excellent stability. It can be used for 100 times with RSDs of extraction efficiency less than 22.4%. The as-established SPME-GC method was applied to determine PAEs in food-wrap and PAHs in cigarette ash and snow water, and satisfactory results were obtained. The carbon nanoparticles-coated SPME fiber was efficient for sampling of organic compounds from aqueous samples.

  2. Electrical and Thermal Behavior of Copper-Epoxy Nanocomposites Prepared via Aqueous to Organic Phase Transfer Technique

    Directory of Open Access Journals (Sweden)

    N. H. Mohd Hirmizi

    2012-01-01

    Full Text Available The preparation, electrical, and thermal behaviors of copper-epoxy nanocomposites are described. Cetyltrimethylammonium bromide- (CTAB- stabilized copper (Cu particles were synthesized via phase transfer technique. Isopropanol (IPA, sodium borohydride (NaBH4, and toluene solution of diglycidyl ether of bisphenol A (DGEBA were used as transferring, reducing agent, and the organic phase, respectively. The UV-Vis absorbance spectra of all the sols prepared indicate that the presence of Cu particles with the particles transfer efficiency is ≥97%. The amount, size, and size distribution of particles in the organosol were dependent on the content of organic solute in the organosol. The composites were obtained upon drying the organosols and these were then subjected to further studies on the curing, thermal, and electrical characteristic. The presence of Cu fillers does not significantly affect the completeness of the composite curing process and only slightly reduce the thermal stability of the composites that is >300°C. The highest conductivity value of the composites obtained is 3.06×10-2 S cm-1.

  3. A mixed-solvent strategy for facile and green preparation of graphene by liquid-phase exfoliation of graphite

    Science.gov (United States)

    Yi, Min; Shen, Zhigang; Ma, Shulin; Zhang, Xiaojing

    2012-08-01

    A versatile and scalable mixed-solvent strategy, by which two mediocre solvents could be combined into good solvents for exfoliating graphite, is demonstrated for facile and green preparation of graphene by liquid-phase exfoliation of graphite. Mild sonication of crystal graphite powder in a mixture of water and alcohol could yield graphene nanosheets, which formed a highly stable suspension in the mixed solvents. The graphene yield was estimated as 10 wt%. The optimum mass fraction of ethanol in water-ethanol mixtures and isopropanol in water-isopropanol mixtures was experimentally determined as 40 and 55 % respectively, which could be roughly predicted by the theory of Hansen solubility parameters. Statistics based on atomic force microscopic analysis show that up to 86 % of the prepared nanosheets were less than 10-layer thick with a monolayer fraction of 8 %. High resolution transmission electron microscopy, infrared spectroscopy, X-ray diffraction, and Raman spectrum analysis of the vacuum-filtered films suggest the graphene sheets to be largely free of defects and oxides. The proposed mixed-solvent strategy here extends the scope for liquid-phase processing graphene and gives researchers great freedom in designing ideal solvent systems for specific applications.

  4. Streamlined Membrane Proteome Preparation for Shotgun Proteomics Analysis with Triton X-100 Cloud Point Extraction and Nanodiamond Solid Phase Extraction

    Directory of Open Access Journals (Sweden)

    Minh D. Pham

    2016-05-01

    Full Text Available While mass spectrometry (MS plays a key role in proteomics research, characterization of membrane proteins (MP by MS has been a challenging task because of the presence of a host of interfering chemicals in the hydrophobic protein extraction process, and the low protease digestion efficiency. We report a sample preparation protocol, two-phase separation with Triton X-100, induced by NaCl, with coomassie blue added for visualizing the detergent-rich phase, which streamlines MP preparation for SDS-PAGE analysis of intact MP and shot-gun proteomic analyses. MP solubilized in the detergent-rich milieu were then sequentially extracted and fractionated by surface-oxidized nanodiamond (ND at three pHs. The high MP affinity of ND enabled extensive washes for removal of salts, detergents, lipids, and other impurities to ensure uncompromised ensuing purposes, notably enhanced proteolytic digestion and down-stream mass spectrometric (MS analyses. Starting with a typical membranous cellular lysate fraction harvested with centrifugation/ultracentrifugation, MP purities of 70%, based on number (not weight of proteins identified by MS, was achieved; the weight-based purity can be expected to be much higher.

  5. Preparation of new hybrid organic/inorganic polymeric chiral stationary phases for ligand-exchange chromatography

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Three new hybrid organic/inorganic polymeric ligand-exchange chiral stationary phases were developed by radical chain transfer reaction and surface grafting on silica gel, and successfully used for the enantioseparations of DL-amino acids and DL-hydroxyl acids. The resolutions were achieved by using water containing 2.0 × 10-4 mol/L of CuAc2 as a mobile phase, column temperature of 40 ℃, flow rate of 1.0 mL/min and detection at UV 254 mn. The elution order of D-isomer before L-isomer was observed for all DL-amino acids resolved except DL-Pro.

  6. Preparation of n-tetradecane-containing microcapsules with different shell materials by phase separation method

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Rui [Department of Chemical Engineering, Tsinghua University, Beijing (China); Zhang, Yan; Zhang, Qingwu [Department of Chemical Engineering, China University of Mining and Technology, Beijing (China); Wang, Xin; Zhang, Yinping [Department of Building Science, Tsinghua University, Beijing (China)

    2009-10-15

    Microcapsules for thermal energy storage and heat-transfer enhancement have attracted great attention. Microencapsulation of n-tetradecane with different shell materials was carried out by phase separation method in this paper. Acrylonitrile-styrene copolymer (AS), acrylonitrile-styrene-butadiene copolymer (ABS) and polycarbonate (PC) were used as the shell materials. The structures, morphologies and the thermal capacities of the microcapsules were characterized using Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The ternary phase diagrams showed the potential encapsulation capabilities of the three shell materials. The effects of the shell/core ratio and the molecular weight of the shell material on the encapsulation efficiency and the thermal capacity of the microcapsules were also discussed. Microcapsules with melting enthalpy > 100 J/g, encapsulation efficiency 66-75%, particle size<1 {mu}m were obtained for all three shell materials. (author)

  7. Relationships between phase morphology and deformation mechanisms in polymer nanocomposite nanofibres prepared by an electrospinning process.

    Science.gov (United States)

    Kim, G M; Lach, R; Michler, G H; Pötschke, P; Albrecht, K

    2006-02-28

    Relationships between phase morphology and mechanical deformation processes in various electrospun polymer nanocomposite nanofibres (PNCNFs) containing different types of one-, two- and three-dimensional nanofiller have been investigated by transmission electron microscopy using in situ tensile techniques. From the study of the phase structure of electrospun PNCNFs, two morphological standard types are classified for the analysis of deformation mechanisms: the binary system (polymer matrix and nanofillers), and the ternary system (polymer matrix, nanofillers and nanopores on the fibres surface). According to these categories, deformation processes have been characterized, and different schematic models for these processes are proposed. The finding of importance in the present work is a brittle-to-ductile transition in polymer nanocomposite fibres during in situ tensile deformation processes. This unique feature in the deformation behaviour of electrospun PNCNFs provides an optimal balance of stiffness, strength and toughness for use as reinforcing elements in a polymer based composite of a new kind.

  8. Copolymerization preparation of cationic cyclodextrin chiral stationary phases for drug enantioseparation in chromatography

    OpenAIRE

    sprotocols

    2015-01-01

    Authors: Ren-Qi Wang, Teng-Teng Ong, Ke Huang, Weihua Tang & Siu-Choon Ng ### Abstract We described a facile and effective protocol wherein radical copolymerization is employed to covalently bond cationic β-cyclodextrin (β-CD) onto silica particles with extended linkage, resulting in a chiral stationary phase (IMPCSP) that can be used for the enantioseparation of racemic drugs in both high-performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC). Start...

  9. Preparation of high-quality poly-Si films by a solid phase crystallizing method

    CERN Document Server

    Yao Ruo He

    2002-01-01

    A solid phase crystallizing method has been developed to grow a Si crystal at temperatures as low as 550 degree C. Using this method, a high-quality thin-film polycrystalline silicon (Poly-Si) was obtained. The largest grain size, examined with X-ray diffraction spectroscopy and scanning electron microscopy images of recrystallized samples, is approximately 1 mu m for substrate temperature at 300 degree C and annealed at 550 degree C for 3 hours

  10. Preparing Future Physics Faculty at the University of Arkansas: Phase I

    Science.gov (United States)

    Stewart, Gay B.

    2000-04-01

    When we embarked upon an NSF supported curriculum development project, it became clear that the first and greatest need for educational reform to be embraced and sustained was for our future faculty to be prepared to be as professional about their roles as educators as their roles as researchers. A new college faculty member may find themselves preparing to teach a class for the first time, with little or no guidance. The biggest complaints employers have about those hired for ``pure" research positions involve interpersonal skills. Also, more researchers are being called upon to do outreach. Teaching and participating in outreach activities develop these skills. Our focus at this stage is to add these kinds of activities to the graduate program, with the same sort of mentoring that accompanies the development of research skills, without extending the time needed to complete a degree. Also, a new masters degree for those that find themselves insufficiently motivated to do research, but still loving physics, provides a route straight into teaching for these students at very low resource cost. Progress made toward these goals so far at the University of Arkansas will be presented.

  11. Liquid-vapor phase diagram and surface properties in oppositely charged colloids represented by a mixture of attractive and repulsive Yukawa potentials.

    Science.gov (United States)

    Chapela, Gustavo A; del Río, Fernando; Alejandre, José

    2013-02-07

    The liquid-vapor phase diagrams of equal size diameter σ binary mixtures of screened potentials have been reported for several ranges of interaction using Monte Carlo simulation methods [J. B. Caballero, A. M. Puertas, A. Ferńandez-Barbero, F. J. de las Nieves, J. M. Romero-Enrique, and L. F. Rull, J. Chem. Phys. 124, 054909 (2006); A. Fortini, A.-P. Hynninen, and M. Dijkstra, J. Chem. Phys. 125, 094502 (2006)]. Both works report controversial results about the stability of the phase diagram with the inverse Debye screening length κ. Caballero found stability for values of κσ up to 20 while Fortini reported stability for κσ up to 20 while Fortini reported stability for κσ ≤ 4. In this work a spinodal decomposition process where the liquid and vapor phases coexist through an interface in a slab geometry is used to obtain the phase equilibrium and surface properties using a discontinuous molecular dynamics simulations for mixtures of equal size particles carrying opposite charge and interacting with a mixture of attractive and repulsive Yukawa potentials at different values of κσ. An crude estimation of the triple point temperatures is also reported. The isothermal-isobaric method was also used to determine the phase stability using one phase simulations. We found that liquid-vapor coexistence is stable for values of κσ > 20 and that the critical temperatures have a maximum value at around κσ = 10, in agreement with Caballero et al. calculations. There also exists a controversy about the liquid-vapor envelope stability of the pure component attractive Yukawa model which is also discussed in the text. In addition, details about the equivalence between continuous and discontinuous molecular dynamics simulations are given, in the Appendix, for Yukawa and Lennard-Jones potentials.

  12. Liquid-vapor phase diagram and surface properties in oppositely charged colloids represented by a mixture of attractive and repulsive Yukawa potentials

    Science.gov (United States)

    Chapela, Gustavo A.; del Río, Fernando; Alejandre, José

    2013-02-01

    The liquid-vapor phase diagrams of equal size diameter σ binary mixtures of screened potentials have been reported for several ranges of interaction using Monte Carlo simulation methods [J. B. Caballero, A. M. Puertas, A. Ferńandez-Barbero, F. J. de las Nieves, J. M. Romero-Enrique, and L. F. Rull, J. Chem. Phys. 124, 054909 (2006), 10.1063/1.2159481; A. Fortini, A.-P. Hynninen, and M. Dijkstra, J. Chem. Phys. 125, 094502 (2006), 10.1063/1.2335453]. Both works report controversial results about the stability of the phase diagram with the inverse Debye screening length κ. Caballero found stability for values of κσ up to 20 while Fortini reported stability for κσ up to 20 while Fortini reported stability for κσ ⩽ 4. In this work a spinodal decomposition process where the liquid and vapor phases coexist through an interface in a slab geometry is used to obtain the phase equilibrium and surface properties using a discontinuous molecular dynamics simulations for mixtures of equal size particles carrying opposite charge and interacting with a mixture of attractive and repulsive Yukawa potentials at different values of κσ. An crude estimation of the triple point temperatures is also reported. The isothermal-isobaric method was also used to determine the phase stability using one phase simulations. We found that liquid-vapor coexistence is stable for values of κσ > 20 and that the critical temperatures have a maximum value at around κσ = 10, in agreement with Caballero et al. calculations. There also exists a controversy about the liquid-vapor envelope stability of the pure component attractive Yukawa model which is also discussed in the text. In addition, details about the equivalence between continuous and discontinuous molecular dynamics simulations are given, in the Appendix, for Yukawa and Lennard-Jones potentials.

  13. Preparation, characterization and application of N-methylene phosphonic acid chitosan grafted magnesia–zirconia stationary phase

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Qing; Chen, Jie; Huang, Kun; Zhang, Xin; Xu, Li [Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030 (China); Shi, Zhi-guo, E-mail: shizg@whu.edu.cn [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2015-01-07

    Highlights: • N-methylene phosphonic acid chitosan grafted MgO–ZrO{sub 2} was prepared. • It exhibited superior HILIC chromatographic performance to the bare MgO–ZrO{sub 2}. • Monosaccharides, phospholipids and peptides were successfully separated. • It was a promising HILIC stationary phase. - Abstract: A hydrophilic stationary phase (SP) was prepared through grafting N-methylene phosphonic acid chitosan on magnesia–zirconia particles (P-CTS-MgO–ZrO{sub 2}) via Lewis acid–base interaction. The resulting material was characterized by thermogravimetric analysis, Fourier transform infrared spectroscopy, scanning electron microscope and nitrogen adsorption analysis. The chromatographic performance of P-CTS-MgO–ZrO{sub 2} was systemically evaluated by studying effect of acetonitrile content, pH and buffer concentration in the mobile phase. The results demonstrated that the novel SP provided hydrophilic, electrostatic-repulsion and ion-exchange interactions. Compared to the bare MgO–ZrO{sub 2}, P-CTS-MgO–ZrO{sub 2} exhibited superior peak shape, reasonable resolution and reduced analysis time in separation of basic analytes. Besides, remarkable resolving power of acids, i.e. six non-steroidal anti-inflammatory drugs which failed to be eluted from the bare MgO–ZrO{sub 2}, was obtained with the theoretical plate number (N/m) of 4653–31313, asymmetry factor <1.21 and the resolution of 1.6–3.4. Finally, P-CTS-MgO–ZrO{sub 2} SP was applied to separate monosaccharides, phospholipids and peptides. P-CTS-MgO–ZrO{sub 2} was a promising hydrophilic SP for wide applications.

  14. Microphase-Separated PE/PEO Thin Films Prepared by Plasma-Assisted Vapor Phase Deposition.

    Science.gov (United States)

    Choukourov, Andrei; Gordeev, Ivan; Ponti, Jessica; Uboldi, Chiara; Melnichuk, Iurii; Vaidulych, Mykhailo; Kousal, Jaroslav; Nikitin, Daniil; Hanyková, Lenka; Krakovský, Ivan; Slavínská, Danka; Biederman, Hynek

    2016-03-01

    Immiscible polymer blends tend to undergo phase separation with the formation of nanoscale architecture which can be used in a variety of applications. Different wet-chemistry techniques already exist to fix the resultant polymeric structure in predictable manner. In this work, an all-dry and plasma-based strategy is proposed to fabricate thin films of microphase-separated polyolefin/polyether blends. This is achieved by directing (-CH2-)100 and (-CH2-CH2-O-)25 oligomer fluxes produced by vacuum thermal decomposition of poly(ethylene) and poly(ethylene oxide) onto silicon substrates through the zone of the glow discharge. The strategy enables mixing of thermodynamically incompatible macromolecules at the molecular level, whereas electron-impact-initiated radicals serve as cross-linkers to arrest the subsequent phase separation at the nanoscale. The mechanism of the phase separation as well as the morphology of the films is found to depend on the ratio between the oligomeric fluxes. For polyolefin-rich mixtures, polyether molecules self-organize by nucleation and growth into spherical domains with average height of 22 nm and average diameter of 170 nm. For equinumerous fluxes and for mixtures with the prevalence of polyethers, spinodal decomposition is detected that results in the formation of bicontinuous structures with the characteristic domain size and spacing ranging between 5 × 10(1) -7 × 10(1) nm and 3 × 10(2)-4 × 10(2) nm, respectively. The method is shown to produce films with tunable wettability and biologically nonfouling properties.

  15. A Fast Algorithm for Phase Grating Preparation by Real Space Method

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Based on a definitely integral formula, an expression ofcalculating atomic potential distribution function U(Υ) in a unit cell is derived as follows: Making use of this expression to calculate the phase grating in high resolution image simulation can greatly reduce the calculating time. In this paper, the derivation of the expression is introduced, and then the computer routine is explained in details. Finally the potential projection map of Mg44Rh7 along [001] direction is shown as an illustration. All operations are carried out in real space, so we call the calculation method as the real space method.

  16. Preparation and characterization of phase change material for thermal energy storage in buildings

    Science.gov (United States)

    Lo, Tommy Y.

    2016-04-01

    The paper presents the developing of novel form-stable composite phase change material (PCM) by incorporation of paraffin into lightweight aggregate through vacuum impregnation. The macro-encapsulated Paraffin-lightweight aggregate is a chemical compatible, thermal stable and thermal reliable PCM material for thermal energy storage applications in buildings. The 28 days compressive strength of NWAC using PCM-LWA is 33 - 53 MPa, which has an opportunity for structural purpose. Scanning electronic microscopic images indicated the paraffin can be held inside the porous structure of the aggregate. Thermal performance test showed that the cement paste panel with composite PCM can reduce the indoor temperature.

  17. Organic molecules modified palladium nanowires arrays prepared by high temperature liquid phase reduction

    Institute of Scientific and Technical Information of China (English)

    Shen Cheng-Min; Yang Tian-Zhong; Xiao Cong-Wen; Zhang Huai-Ruo; Tian Ji-Fa; Bao Li-Hong; Li Chen; Li Jian-Qi; Gao Hong-Jun

    2008-01-01

    This paper reports high temperature liquid phase synthesis of Pd nanowires using chemically modified porous anodic aluminium oxide as template. In this synthesis process, oleic acid is used to modify the inner wall of the pores and Pd2+ complex with oleylamine is filled into the channel of the template. The complex is then reduced to give oleylamine-capped Pd nanowires. This paper suggests that oleic acid can improve the environment of inner wall of the pores, leading to the formation of uniform Pd nanowires. The synthetic process can be extended to make other types of nanowires.

  18. A novel bio-safe phase separation process for preparing open-pore biodegradable polycaprolactone microparticles.

    Science.gov (United States)

    Salerno, Aurelio; Domingo, Concepción

    2014-09-01

    Open-pore biodegradable microparticles are object of considerable interest for biomedical applications, particularly as cell and drug delivery carriers in tissue engineering and health care treatments. Furthermore, the engineering of microparticles with well definite size distribution and pore architecture by bio-safe fabrication routes is crucial to avoid the use of toxic compounds potentially harmful to cells and biological tissues. To achieve this important issue, in the present study a straightforward and bio-safe approach for fabricating porous biodegradable microparticles with controlled morphological and structural features down to the nanometer scale is developed. In particular, ethyl lactate is used as a non-toxic solvent for polycaprolactone particles fabrication via a thermal induced phase separation technique. The used approach allows achieving open-pore particles with mean particle size in the 150-250 μm range and a 3.5-7.9 m(2)/g specific surface area. Finally, the combination of thermal induced phase separation and porogen leaching techniques is employed for the first time to obtain multi-scaled porous microparticles with large external and internal pore sizes and potential improved characteristics for cell culture and tissue engineering. Samples were characterized to assess their thermal properties, morphology and crystalline structure features and textural properties.

  19. Porous Polyimide Membranes Prepared by Wet Phase Inversion for Use in Low Dielectric Applications

    Directory of Open Access Journals (Sweden)

    Jung Ah Lim

    2013-04-01

    Full Text Available A wet phase inversion process of polyamic acid (PAA allowed fabrication of a porous membrane of polyimide (PI with the combination of a low dielectric constant (1.7 and reasonable mechanical properties (Tensile strain: 8.04%, toughness: 3.4 MJ/m3, tensile stress: 39.17 MPa, and young modulus: 1.13 GPa, with further thermal imidization process of PAA. PAA was simply synthesized from purified pyromellitic dianhydride (PMDA and 4,4-oxydianiline (ODA in two different reaction solvents such as γ-butyrolactone (GBL and N-methyl-2-pyrrolidinone (NMP, which produce Mw/PDI of 630,000/1.45 and 280,000/2.0, respectively. The porous PAA membrane was fabricated by the wet phase inversion process based on a solvent/non-solvent system via tailored composition between GBL and NMP. The porosity of PI, indicative of a low electric constant, decreased with increasing concentration of GBL, which was caused by sponge-like formation. However, due to interplay between the low electric constant (structural formation and the mechanical properties, GBL was employed for further exploration, using toluene and acetone vs. DI-water as a coagulation media. Non-solvents influenced determination of the PAA membrane size and porosity. With this approach, insight into the interplay between dielectric properties and mechanical properties will inform a wide range of potential low-k material applications.

  20. Preparation of Medium Cation Exchange Stationary Phase of Polymeric Matrix and Their Chromatographic Properties

    Institute of Scientific and Technical Information of China (English)

    CHEN,Gang; GONG,Bo-Lin; BAI,Quan; GENG,Xin-Du

    2007-01-01

    Based on the monodisperse poly(glycidyl methacrylate-co-ethylenedimethacrylate) beads (PGMA/EDMA) with macropore as a medium, a new hydrophilic medium cation exchange (MCX) stationary phase for HPLC was synthesized by a new chemically modified method. The stationary phase was evaluated with the property of ion exchange, separability, reproducibility, hydrophilicity, effect of salt concentration, salt types, column loading and pH on the separation and retention of proteins in detail. It was found that it follows ion exchange chromatographic (IEC)retention mechanism. The measured bioactivity recovery for lysozyme was (96±5)%. The dynamic protein loading capacity of the synthesized MCX packings was 21.8 mg/g. Five proteins were almost completely separated within 6.0 min at a flow rate of 4 mL/min using the synthesized MCX resin. The MCX resin was also used for the rapid separation and purification of lysozyme from egg white with only one step. The purity and specific bioactivity of the purified lysozyme was found more than 95% and 70345 U/mg, respectively.

  1. Preparation of Nb3Al superconductor by powder metallurgy and effect of mechanical alloying on the phase formation

    Institute of Scientific and Technical Information of China (English)

    Zhao Liu; Yongliang Chen; Lupeng Du; Pingyuan Li; Yajing Cui; Xifeng Pan; Guo Yan

    2014-01-01

    Adoption of powder-in-tube method to fabri-cate superconducting wire can realize a large application of Nb3Al prepared by powder metallurgy. Powder metallurgy was used to synthesize Nb3Al under various heat-treatment conditions, annealing temperature was varied from 700 to 1,000 ?C and heating time was varied from 10 to 50 h. X-ray diffraction patterns reveal that a reaction between Nb and Al took place and formed NbAl3 phase. Under current heat-treatment conditions (annealing temperature was varied from 700 to 1,000 ?C and heating time was varied from 10 to 50 h), NbAl3 was so stable that it did not further react with the unreacted Nb and was not sensitive to the heat-treatment condition. By mechanical alloying, adoption of high-energy ball milling significantly decreases particle size and enhances surface free energy, which promotes the formation of Nb3Al phase. X-ray diffraction patterns indicate that relatively pure Nb3Al phase was obtained under the same heat-treatment condition. Energy-disper-sive X-ray analysis measurement demonstrates that the obtained samples were close to the right stoichiometry of A15 structure Nb3Al.

  2. Complexation-Induced Phase Separation: Preparation of Metal-Rich Polymeric Membranes

    KAUST Repository

    Villalobos Vazquez de la Parra, Luis Francisco

    2017-08-01

    The majority of state-of-the-art polymeric membranes for industrial or medical applications are fabricated by phase inversion. Complexation induced phase separation (CIPS)—a surprising variation of this well-known process—allows direct fabrication of hybrid membranes in existing facilities. In the CIPS process, a first step forms the thin metal-rich selective layer of the membrane, and a succeeding step the porous support. Precipitation of the selective layer takes place in the same solvent used to dissolve the polymer and is induced by a small concentration of metal ions. These ions form metal-coordination-based crosslinks leading to the formation of a solid skin floating on top of the liquid polymer film. A subsequent precipitation in a nonsolvent bath leads to the formation of the porous support structure. Forming the dense layer and porous support by different mechanisms while maintaining the simplicity of a phase inversion process, results in unprecedented control over the final structure of the membrane. The thickness and morphology of the dense layer as well as the porosity of the support can be controlled over a wide range by manipulating simple process parameters. CIPS facilitates control over (i) the thickness of the dense layer throughout several orders of magnitude—from less than 15 nm to more than 6 μm, (ii) the type and amount of metal ions loaded in the dense layer, (iii) the morphology of the membrane surface, and (iv) the porosity and structure of the support. The nature of the CIPS process facilitates a precise loading of a high concentration of metal ions that are located in only the top layer of the membrane. Moreover, these metal ions can be converted—during the membrane fabrication process—to nanoparticles or crystals. This simple method opens up fascinating possibilities for the fabrication of metal-rich polymeric membranes with a new set of properties. This dissertation describes the process in depth and explores promising

  3. Preparations of Pure Alkaline Earth Molybdate Phases from Single Molecular Precursors

    Institute of Scientific and Technical Information of China (English)

    JIANG Ya-qi; ZHAO Hong; FANG Zhi-min; WAN Hui-lin; XIONG Ming; ZHOU Zhao-hui

    2004-01-01

    The pure phases of alkaline earth molybdates MMoO4, where M=Mg, Ca, Sr or Ba, were synthesized via the calcination of the related citrato oxomolybdate complexes. The mixed metal oxides can be highly dispersed at the atomic level due to the existence of uniform citrato oxomolybdenum precursors in definite composition. The complexing effect helps to produce the fine-grained oxides with particle size in the ultrafine scale(<100 nm) at heat-treatment temperatures below 500 ℃. The structures of the precursor complexes and the finally heat-treated particles were studied by means of IR, XRD, DSC, DTA and TG techniques. The morphologies of the particles were observed by using the SEM technique. The average particle sizes were calculated to be in the range of 30-50 nm based on X-ray diffraction line-broadening and SEM images, indicating the poor conglomeration of crystallite at low temperatures.

  4. Characterization of Bimetallic Fe-Ru Oxide Nanoparticles Prepared by Liquid-Phase Plasma Method

    Science.gov (United States)

    Lee, Sung-Jin; Lee, Heon; Jeon, Ki-Joon; Park, Hyunwoong; Park, Young-Kwon; Jung, Sang-Chul

    2016-07-01

    The bimetallic Fe-Ru oxide nanoparticles were synthesized in the liquid-phase plasma (LPP) method which employed iron chloride and ruthenium chloride as precursors. The active species (OH·, Hα, Hβ, and OI) and the iron and ruthenium ions were observed in the plasma field created by the LPP process. The spherical-shaped bimetallic Fe-Ru oxide nanoparticles were synthesized by the LPP reaction, and the size of the particles was growing along with the progression of the LPP reaction. The synthesized bimetallic Fe-Ru oxide nanoparticles were comprised of Fe2O3, Fe3O4, RuO, and RuO2. Ruthenium had a higher reduction potential than iron and resulted in higher ruthenium composition in the synthesized bimetallic nanoparticles. The control of the molar ratio of the precursors in the reactant solution was found to be employed as a means to control the composition of the elements in bimetallic nanoparticles.

  5. Dopamine/TiO{sub 2} hybrid thin films prepared by the liquid phase deposition method

    Energy Technology Data Exchange (ETDEWEB)

    Gutierrez-Tauste, David [Departament de Quimica, Universitat Autonoma de Barcelona, Campus UAB, Edifici Cn, 08290 Cerdanyola del Valles, Barcelona (Spain)], E-mail: davidg@qf.uab.es; Domenech, Xavier [Departament de Quimica, Universitat Autonoma de Barcelona, Campus UAB, Edifici Cn, 08290 Cerdanyola del Valles, Barcelona (Spain); Domingo, Concepcion [Instituto de Ciencia de Materiales (CSIC), Campus UAB, 08290 Cerdanyola del Valles, Barcelona (Spain); Ayllon, Jose A. [Departament de Quimica, Universitat Autonoma de Barcelona, Campus UAB, Edifici Cn, 08290 Cerdanyola del Valles, Barcelona (Spain)

    2008-04-30

    Liquid phase deposition method is applied to one-step production of a hybrid material composed by dopamine(DA) and TiO{sub 2} anatase. An optimized amount of the enediol derivative is added to a fluoride titania precursor aqueous solution in order to entrap this modifier within the growing TiO{sub 2}, yielding a DA/TiO{sub 2} nanocomposite material. Uniform, well-adhered and brown-colored thin films are deposited on indium tin oxide covered glass substrate. The DA/TiO{sub 2} hybrid material has been characterized by infrared spectroscopy, electronic microscopy, X-ray diffraction and UV-vis spectroscopy. The formation of the hybrid material seems to be reasonably explained by linkage of different TiO{sub 2} nanocrystallites taking advantage of both enediol and amine groups of DA.

  6. Colocalization and interaction between elongasome and divisome during a preparative cell division phase in Escherichia coli.

    Science.gov (United States)

    van der Ploeg, René; Verheul, Jolanda; Vischer, Norbert O E; Alexeeva, Svetlana; Hoogendoorn, Eelco; Postma, Marten; Banzhaf, Manuel; Vollmer, Waldemar; den Blaauwen, Tanneke

    2013-03-01

    The rod-shaped bacterium Escherichia coli grows by insertion of peptidoglycan into the lateral wall during cell elongation and synthesis of new poles during cell division. The monofunctional transpeptidases PBP2 and PBP3 are part of specialized protein complexes called elongasome and divisome, respectively, which catalyse peptidoglycan extension and maturation. Endogenous immunolabelled PBP2 localized in the cylindrical part of the cell as well as transiently at midcell. Using the novel image analysis tool Coli-Inspector to analyse protein localization as function of the bacterial cell age, we compared PBP2 localization with that of other E. coli cell elongation and division proteins including PBP3. Interestingly, the midcell localization of the two transpeptidases overlaps in time during the early period of divisome maturation. Försters Resonance Energy Transfer (FRET) experiments revealed an interaction between PBP2 and PBP3 when both are present at midcell. A decrease in the midcell diameter is visible after 40% of the division cycle indicating that the onset of new cell pole synthesis starts much earlier than previously identified by visual inspection. The data support a new model of the division cycle in which the elongasome and divisome interact to prepare for cell division.

  7. Comparison of preparative reversed phase liquid chromatography and countercurrent chromatography for the kilogram scale purification of crude spinetoram insecticide.

    Science.gov (United States)

    DeAmicis, Carl; Edwards, Neil A; Giles, Michael B; Harris, Guy H; Hewitson, Peter; Janaway, Lee; Ignatova, Svetlana

    2011-09-09

    Reversed phase HPLC (RP-HPLC) and high performance countercurrent chromatography (HPCCC) were compared for the pilot scale purification of two semi-synthetic spinosyns, spinetoram-J and spinetoram-L, the major components of the commercial insecticide spinetoram. Two, independently performed, 1 kg, purification campaigns were compared. Each method resulted in the isolation of both components at a purity of >97% and yields for spinetoram-J and spinetoram-L of >93% and ≥ 63% of theoretical, respectively. The HPCCC process produced a 2-fold higher throughput and consumed approximately 70% less solvent than preparative scale RP-HPLC, the volume of product containing fractions from HPCCC amounted to 7% of that produced by HPLC and so required much less post-run processing.

  8. Low power optical limiting studies on nanocrystalline benzimidazole thin films prepared by modified liquid phase growth technique

    Indian Academy of Sciences (India)

    P A Praveen; S P Prabhakaran; R Ramesh Babu; K Sethuraman; K Ramamurthi

    2015-06-01

    In the present work, benzimidazole (BMZ), a well known nonlinear optical material, thin films were deposited using the modified liquid phase growth technique at different solution temperatures. The prepared samples were subjected to spectral, structural and surface analyses. Linear optical properties and third-order optical nonlinearity of the deposited BMZ thin films were analysed using UV–visible–NIR spectrum and -scan technique, respectively. The experimental results show that the BMZ films exhibit reverse saturable absorption and positive nonlinearity at 650 nm CW laser of power 5 mW. The measured third-order nonlinear susceptibility of the films is about 10−10 esu. Optical limiting studies were performed using the same laser source and the potentiality of the BMZ films is reported.

  9. Preparation of Freestanding GaN Wafers by Hydride Vapor Phase Epitaxy with Void-Assisted Separation

    Science.gov (United States)

    Oshima, Yuichi; Eri, Takeshi; Shibata, Masatomo; Sunakawa, Haruo; Kobayashi, Kenji; Ichihashi, Toshinari; Usui, Akira

    2003-01-01

    We have developed a novel technique for preparing large-scale freestanding GaN wafers. Hydride vapor phase epitaxy (HVPE) growth of thick GaN layer was performed on a GaN template with a thin TiN film on the top. After the cooling process of the HVPE growth, the thick GaN layer was easily separated from the template by the assistance of many voids generated around the TiN film. As a result, a freestanding GaN wafer was obtained. The wafer obtained had a diameter of 45 mm, and a mirror-like surface. The-full-width-at-half-maximum (FWHM) of (0002) and (10\\bar{1}0) peaks in the X-ray rocking curve profile were 60 and 92 arcsec, respectively. The dislocation density was evaluated at 5× 106 cm-3 by etch pit density measurement.

  10. Kinetics and thermodynamics of basic dye sorption on phosphoric acid esterifying soybean hull with solid phase preparation technique.

    Science.gov (United States)

    Gong, Renmin; Sun, Jin; Zhang, Demin; Zhong, Keding; Zhu, Guoping

    2008-07-01

    In this paper, the solid phase preparation method of a cationic sorbent, which bears hydroxyl groups of phosphoric acid derived from esterified soybean hull (ESH), was reported. The sorption kinetics and thermodynamics of two basic dyes, acridine orange (AO) and malachite green (MG), from aqueous solution onto ESH were investigated with a batch system. The isothermal data of dye sorptions followed the Langmuir model better than the Freundlich model. The maximum sorption capacity (Q(m)) of ESH for AO and MG was 238.1 mg/g and 178.57 mg/g, respectively. The dye sorption processes could be described by the pseudo-second-order kinetic model. The thermodynamic study indicated that the dye sorptions were spontaneous and exothermic. Lower temperatures were favorable for the sorption processes.

  11. Monitoring preparation and phase transitions of carburized W(1 1 0) by reflectance difference spectroscopy.

    Science.gov (United States)

    Bachmann, Magdalena; Memmel, Norbert; Bertel, Erminald; Denk, Mariella; Hohage, Michael; Zeppenfeld, Peter

    2012-10-01

    Reflectance difference spectroscopy (RDS) is applied to follow in situ the preparation of clean and carburized W(1 1 0) surfaces and to study the temperature-induced transition between the R(15 × 3) and R(15 × 12) carbon/tungsten surface phases. RDS data for this transition are compared to data obtained from Auger-electron spectroscopy and low-energy electron diffraction. All techniques reveal that this transition, occurring around 1870 K, is reversible with a small hysteresis, indicating a first-order-like behaviour. The present results also prove a high surface sensitivity of RDS, which is attributed to the excitation of electronic p-like surface resonances of W(1 1 0).

  12. Preparation of urea-formaldehyde paraffin microcapsules modified by carboxymethyl cellulose as a potential phase change material

    Institute of Scientific and Technical Information of China (English)

    Zhan-hua Huang; Xin Yu; Wei Li; Shou-xin Liu

    2015-01-01

    We prepared spherical microcapsules modified by carboxymethyl cellulose (CMC) with urea-formalde-hyde (UF) resin as a shell material with a two-step process by in situ polymerization, and characterized the micro-cosmic features, chemical structure, and thermal perfor-mance of the microcapsules by SEM, FTIR, DSC, and TGA. We studied the effects of different experimental parameters of curing pH, the amounts of the emulsifier and emulsion speed. The CMC-UF microcapsules had good heat resistance and stability. The enthalpy of CMC-UF microcapsules reached 50.33 J g-1. Therefore, CMC-UF resin can be used as a potential wall material of phase change materials.

  13. Preparation of hybrid thiol-acrylate emulsion-templated porous polymers by interfacial copolymerization of high internal phase emulsions.

    Science.gov (United States)

    Langford, Caitlin R; Johnson, David W; Cameron, Neil R

    2015-05-01

    Emulsion-templated highly porous polymers (polyHIPEs), containing distinct regions differing in composition, morphology, and/or properties, are prepared by the simultaneous polymerization of two high internal phase emulsions (HIPEs) contained within the same mould. The HIPEs are placed together in the mould and subjected to thiol-acrylate photopolymerization. The resulting polyHIPE material is found to contain two distinct semicircular regions, reflecting the composition of each HIPE. The original interface between the two emulsions becomes a copolymerized band between 100 and 300 μm wide, which is found to be mechanically robust. The separate polyHIPE layers are distinguished from one another by their differing average void diameter, chemical composition, and extent of contraction upon drying.

  14. Facile preparation and applications of graphitic carbon nitride coating in solid-phase microextraction.

    Science.gov (United States)

    Xu, Na; Wang, Yiru; Rong, Mingcong; Ye, Zhifeng; Deng, Zhuo; Chen, Xi

    2014-10-17

    In this study, graphitic carbon nitride (g-C3N4) was used as a coating material for solid-phase microextraction (SPME) applications. Coupled to gas chromatography (GC), the extraction ability of the SPME fiber was investigated and compared with the commercial fibers of 100 μm PDMS and 85 μm CAR/PDMS using six target analytes including deltamethrin, nerolidol, amphetamine, dodecane, ametryn and acrylamide. The g-C3N4 coating revealed excellent extraction ability and durability comparing with those of the commercial fibers due to its loose structure and unique physicochemical properties. The repeatability for each single fiber was found to be 3.46% and reproducibility for fiber to fiber was 8.53%. The g-C3N4 SPME fiber was applied to the determination of acrylamide in potato chips, the linearity and detection limit was 0.5-250 μg g(-1) and 0.018 μg g(-1), respectively.

  15. PREPARATION OF POROUS NANOCOMPOSITE SCAFFOLDS WITH HONEYCOMB MONOLITH STRUCTURE BY ONE PHASE SOLUTION FREEZE DRYING METHOD

    Institute of Scientific and Technical Information of China (English)

    Yang Xu; Duo Zhang; Zong-liang Wang; Zhan-tuan Gao; Pei-biao Zhang; Xue-si Chen

    2011-01-01

    Biodegradable porous nanocomposite scaffolds of poly(lactide-co-glycolide) (PLGA) and L-lactic acid (LAc) oligomer surface-grafted hydroxyapatite nanoparticles (op-HA) with a honeycomb monolith structure were fabricated with the single-phase solution freeze-drying method. The effects of different freezing temperatures on the properties of the scaffolds, such as microstructures, compressive strength, cell penetration and cell proliferation were studied. The highly porous and well interconnected scaffolds with a tunable pore structure were obtained. The effect of different freezing temperature (4℃, -20℃, -80℃ and -196℃) was investigated in relation to the scaffold morphology, the porosity varied from 91.2% to 83.0% and the average pore diameter varied from (167.2 ± 62.6) pm to (11.9 ± 4.2) μm while the σ10 increased significantly. The cell proliferation were decreased and associated with the above-mentioned properties. Uniform distribution of op-HA particles and homogeneous roughness of pore wall surfaces were found in the 4℃ frozen scaffold. The 4℃ frozen scaffold exhibited better cell penetration and increased cell proliferation because of its larger pore size, higher porosity and interconnection. The microstmctures described here provide a new approach for the design and fabrication of op-HA/PLGA based scaffold materials with potentially broad applicability for replacement of bone defects.

  16. Antioxidative properties of defatted dabai pulp and peel prepared by solid phase extraction.

    Science.gov (United States)

    Khoo, Hock Eng; Azlan, Azrina; Ismail, Amin; Abas, Faridah

    2012-08-14

    Solid phase extraction (SPE) using Sep-Pak® cartridges is one of the techniques used for fractionation of antioxidant compounds in waste of dabai oil extraction (defatted dabai parts). The aim of this study was to determine the phenolic compounds and antioxidant capacity in crude extracts and several SPE fractions from methanolic extract of defatted dabai pulp and peel. Based on SPE, Sep-Pak® cyanopropyl and C₁₈ cartridges were used to fractionate the antioxidant-rich crude extracts into water and methanolic fractions. Analyzed using LC-MS, flavonoids, anthocyanins, saponin derivatives and other unknown antioxidative compounds were detected in the defatted dabai crude extracts and their SPE fractions. Anthocyanins were the major phenolic compounds identified in the defatted dabai peel and detected in most of the SPE fractions. Methanolic fractions of defatted dabai parts embraced higher total phenolics and antioxidant capacity than water fractions. This finding also revealed the crude extracts of defatted dabai peel have the most significant antioxidant properties compared to the methanolic and water fractions studied. The crude extract of defatted dabai parts remain as the most potent antioxidant as it contains mixture of flavonoids, anthocyanins and other potential antioxidants.

  17. Effect Anticipation Affects Perceptual, Cognitive, and Motor Phases of Response Preparation: Evidence from an Event-Related Potential (ERP) Study.

    Science.gov (United States)

    Harrison, Neil R; Ziessler, Michael

    2016-01-01

    The anticipation of action effects is a basic process that can be observed even for key-pressing responses in a stimulus-response paradigm. In Ziessler et al.'s (2012) experiments participants first learned arbitrary effects of key-pressing responses. In the test phase an imperative stimulus determined the response, but participants withheld the response until a Go-stimulus appeared. Reaction times (RTs) were shorter if the Go-stimulus was compatible with the learned response effect. This is strong evidence that effect representations were activated during response planning. Here, we repeated the experiment using event-related potentials (ERPs), and we found that Go-stimulus locked ERPs depended on the compatibility relationship between the Go-stimulus and the response effect. In general, this supports the interpretation of the behavioral data. More specifically, differences in the ERPs between compatible and incompatible Go-stimuli were found for the early perceptual P1 component and the later frontal P2 component. P1 differences were found only in the second half of the experiment and for long stimulus onset asynchronies (SOAs) between imperative stimulus and Go-stimulus, i.e., when the effect was fully anticipated and the perceptual system was prepared for the effect-compatible Go-stimulus. P2 amplitudes, likely associated with evaluation and conflict detection, were larger when Go-stimulus and effect were incompatible; presumably, incompatibility increased the difficulty of effect anticipation. Onset of response-locked lateralized readiness potentials (R-LRPs) occurred earlier under incompatible conditions indicating extended motor processing. Together, these results strongly suggest that effect anticipation affects all (i.e., perceptual, cognitive, and motor) phases of response preparation.

  18. Preparation and Thermal Characterization of Nitrates/Expanded Graphite Composite Phase-Change Material for Thermal Energy Storage

    Science.gov (United States)

    Li, Y.; Li, P.; Zhu, Q. Z.; Li, Q. F.

    2016-11-01

    Molten nitrate is widely used as thermal storage medium in the solar thermal power plants for its appropriate phase-change temperature, high heat storage density and low cost, etc. But its low thermal conductivity, heat absorbing and releasing rate limited its application. Expanded graphite (EG) can compensate the low thermal conductivity of nitrate. In this study, binary nitrates at the weight ratio of 4:6 for LiNO3:KNO3 were prepared using static mixed melting method. EG with the mass fraction of 5 %, 10 %, 15 %, 20 % and 30 % was used to enhance the thermal conductivity. The compound of nitrates/EG was prepared using the ultrasonic smashing method. The thermal conductivity of binary nitrates, EG and nitrates/EG composite was measured by the transient plane heat source technique (TPS). The thermal behaviors were analyzed with a differential scanning calorimeter (DSC). Results showed that the addition of EG significantly enhanced the thermal conductivity, e.g., the thermal conductivity of 10 wt% EG composite phase-change material (PCM) is 8.5 W(m{^{-1}} K{^{-1}}) to 9.5 W(m{^{-1}}K{^{-1}}), which is about eight times larger than that of binary nitrates. To observe the combination morphology, pure EG, nitrates/EG composite PCM and binary nitrates were characterized using scanning electron microscope (SEM). The thermal reliability of the binary nitrates and the composite PCM was determined by DSC. Thermal cycling test showed that both binary nitrates and nitrates/EG composite material have good thermal reliability.

  19. A versatile polydopamine platform for facile preparation of protein stationary phase for chip-based open tubular capillary electrochromatography enantioseparation.

    Science.gov (United States)

    Liu, Chun-Ming; Liang, Ru-Ping; Wang, Xiao-Ni; Wang, Jing-Wu; Qiu, Jian-Ding

    2013-06-14

    A novel, simple, and economical method for the preparation of chiral stationary phases for chip-based enantioselective open tubular capillary electrochromatography (OT-CEC) using polydopamine (PDA) coating as an adhesive layer was reported for the first time. After the poly(dimethylsiloxane) (PDMS) microfluidic chip was filled with dopamine (DA) solution, PDA film was gradually formed and deposited on the inner wall of microchannel as permanent coating via the oxidation of DA by the oxygen dissolved in the solution. Due to possessing plentiful catechol and amine functional groups, PDA coating can serve as a versatile multifunctional platform for further secondary reactions, leading to tailoring of the coatings for protein bioconjugation by the thiols and amines via Michael addition or Schiff base reactions. Bovine serum albumin (BSA), acting as a target protein, was then stably and homogeneously immobilized in the PDA-coated PDMS microchannel to fabricate a novel protein stationary phase. Compared with the native PDMS microchannels, the modified surfaces exhibited much better wettability, more stable and enhanced electroosmotic mobility, and less nonspecific adsorption. The water contact angle and electroosmotic flow of PDA/BSA-coated PDMS substrate were measured to be 44° and 2.83×10(-4)cm(2)V(-1)s(-1), compared to those of 112° and 2.10×10(-4)cm(2)V(-1)s(-1) from the untreated one, respectively. Under a mild condition, d- and l-tryptophan were efficiently separated with a resolution of 1.68 within 130s utilizing a separation length of 37mm coupled with in-column amperometric detection on the PDA/BSA-coated PDMS microchips. This present versatile platform, facile conjugation of biomolecules onto microchip surfaces via mussel adhesive protein inspired coatings, may offer new processing strategies to prepare a biomimetic surface design on microfluidic chips, which is promising in high-throughput and complex biological analysis. Copyright © 2013 Elsevier B

  20. Effect anticipation affects perceptual, cognitive, and motor phases of response preparation: evidence from an event-related potential (ERP study

    Directory of Open Access Journals (Sweden)

    Neil Richard Harrison

    2016-01-01

    Full Text Available The anticipation of action effects is a basic process that can be observed even for key-pressing responses in a stimulus-response paradigm. In Ziessler, Nattkemper and Vogt’s (2012 experiments participants first learned arbitrary effects of key-pressing responses. In the test phase an imperative stimulus determined the response, but participants withheld the response until a Go-stimulus appeared. Reaction times were shorter if the Go-stimulus was compatible with the learned response effect. This is strong evidence that effect representations were activated during response planning. Here we repeated the experiment using event-related potentials (ERPs, and we found that Go-stimulus locked ERPs depended on the compatibility relationship between the Go-stimulus and the response effect. In general, this supports the interpretation of the behavioural data. More specifically, differences in the ERPs between compatible and incompatible Go-stimuli were found for the early perceptual P1 component and the later frontal P2 component. P1 differences were found only in the second half of the experiment and for long SOAs between imperative stimulus and Go-stimulus, i.e. when the effect was fully anticipated and the perceptual system was prepared for the effect-compatible Go-stimulus. P2 amplitudes, likely associated with evaluation and conflict detection, were larger when Go-stimulus and effect were incompatible; presumably, incompatibility increased the difficulty of effect anticipation. Onset of response-locked LRPs occurred earlier under incompatible conditions indicating extended motor processing. Together, these results strongly suggest that effect anticipation affects all (i.e. perceptual, cognitive, and motor phases of response preparation.

  1. Effect of kaolin particle size and loading on the characteristics of kaolin ceramic support prepared via phase inversion technique

    Directory of Open Access Journals (Sweden)

    Siti Khadijah Hubadillah

    2016-06-01

    Full Text Available In this study, low cost ceramic supports were prepared from kaolin via phase inversion technique with two kaolin particle sizes, which are 0.04–0.6 μm (denoted as type A and 10–15 μm (denoted as type B, at different kaolin contents ranging from 14 to 39 wt.%, sintered at 1200 °C. The effect of kaolin particle sizes as well as kaolin contents on membrane structure, pore size distribution, porosity, mechanical strength, surface roughness and gas permeation of the support were investigated. The support was prepared using kaolin type A induced asymmetric structure by combining macroporous voids and sponge-like structure in the support with pore size of 0.38 μm and 1.05 μm, respectively, and exhibited ideal porosity (27.7%, great mechanical strength (98.9 MPa and excellent gas permeation. Preliminary study shows that the kaolin ceramic support in this work is potential to gas separation application at lower cost.

  2. Preparation of 4-butylaniline-bonded silica gel for the solid-phase extraction of flavone glycosides.

    Science.gov (United States)

    Chu, Ganghui; Cai, Wensheng; Shao, Xueguang

    2015-04-01

    To extract flavone glycosides efficiently, a new extraction material based on 4-butylaniline-bonded silica gel was prepared using a two-step grafting method including a ring-opening reaction and synchronous hydrolysis. Preparation of the silica-based material was easily achieved under mild conditions, and the material was characterized by Fourier transform infrared spectroscopy, elemental analysis, and scanning electron microscopy. The material was used in solid-phase extraction, and the extraction can be performed in neutral conditions without regard to ionic strength. Selectivity tests of 14 compounds on the extraction cartridge showed that the material has a high affinity to flavone glycosides in contrast to octadecyl silica, and the extraction yields for four flavone glycosides were found to be >93%. Selectivity tests further reveal that the adsorption on its surface is likely attributed to multiple interactions, including hydrophobic interactions, π-π interactions, and hydrogen bonding. To explore the applicability of 4-butylaniline-bonded silica gel, naringin and hesperidin from Simotang oral liquid were extracted, and the extraction yields were >90%, which is distinguished from silica cartridge.

  3. Preparation, thermal properties and thermal reliability of microencapsulated n-eicosane as novel phase change material for thermal energy storage

    Energy Technology Data Exchange (ETDEWEB)

    Alkan, Cemil; Sari, Ahmet; Karaipekli, Ali [Department of Chemistry, Gaziosmanpasa University, 60240 Tokat (Turkey)

    2011-01-15

    This study deals with preparation, characterization, thermal properties and thermal reliability of n-eicosane microcapsules as novel phase change material (PCM) for thermal energy storage. The microcapsulated PCMs were prepared by coating n-eicosane with polymethylmethacrylate (PMMA) shell. Fourier transform infrared (FT-IR), scanning electron microscope (SEM) and particle size distribution (PSD) analysis were used to characterize the PMMA/eicosane microcapsules as microcapsulated PCMs. The PSD analysis indicated that the average diameter of microcapsules was found to be 0.70 {mu}m under the stirring speed of 2000 rpm. Thermal properties and thermal reliability of the microcapsules were determined using differential scanning calorimetry (DSC) and thermo gravimetric analysis (TGA) methods. From DSC analysis, the melting and freezing temperatures and the latent heats of the microcapsules were measured as 35.2 C and 34.9 C, 84.2 and -87.5 J/g, respectively. TGA analysis indicated that PMMA/eicosane microcapsules degrade in three steps at considerably high temperatures. Accelerated thermal cycling tests have been also applied to show the thermal reliability of the microcapsules. All results showed that thermal properties make the PMMA/eicosane microcapsules potential PCM for thermal energy storage. (author)

  4. Preparation and properties of polystyrene encapsulated paraffin wax as possible phase change material in a polypropylene matrix

    Energy Technology Data Exchange (ETDEWEB)

    Mochane, M.J. [Department of Chemistry, University of the Free State (Qwaqwa Campus), Phuthaditjhaba (South Africa); Luyt, A.S., E-mail: LuytAS@qwa.ufs.ac.za [Department of Chemistry, University of the Free State (Qwaqwa Campus), Phuthaditjhaba (South Africa)

    2012-09-20

    Highlights: Black-Right-Pointing-Pointer Polystyrene microcapsules containing about 30 wt% soft paraffin wax were successfully prepared. Black-Right-Pointing-Pointer The presence of microcapsules in polypropylene influenced the morphology and properties of the matrix. Black-Right-Pointing-Pointer The SEBS modifier had little influence on the interaction between polypropylene and microcapsules. - Abstract: The study deals with the preparation and characterization of polystyrene (PS) capsules containing Fischer-Tropsch paraffin wax (PS:wax) as phase change material (PCM) for thermal energy storage embedded in a polypropylene (PP) matrix. Blends of PP/PS:wax were prepared without and with polystyrene-block-poly(ethylene-ran-butylene)-block-polystyrene (SEBS) as a modifier. The influence of PS:wax microcapsules on the morphology, as well as thermal and mechanical properties of the PP was investigated. The scanning electron microscopy (SEM) images of the microencapsulated PCM show that the capsules were grouped in irregular spherical agglomerates of size 16-24 {mu}m. However, after melt-blending with PP smaller, perfectly spherical microcapsules were well dispersed in the PP matrix. There was fairly good interaction between the microcapsules and the matrix, even in the absence of SEBS modification. The FTIR spectrum of the microcapsules is almost exactly the same as that of polystyrene, which indicates that the microcapsules were mostly intact and that the FTIR only detected the polystyrene shell. The amount of wax in the PS:wax microcapsules was determined as 20-30% by weight. An increase in PS:wax content resulted in a decrease in the melting peak temperatures of PP. The thermal stability of the blends decreased with an increase in PS:wax microcapsules content as a consequence of the lower thermal stability of both the wax and PS. There was a drop in storage modulus with increasing PS:wax microcapsules content.

  5. Aging dependent phase transformation of mesostructured titanium dioxide nanomaterials prepared by evaporation-induced self-assembly process: Implications for solar hydrogen production

    Directory of Open Access Journals (Sweden)

    Luther Mahoney

    2015-08-01

    Full Text Available Mesostructured titanium dioxide materials were prepared by Evaporation-Induced Self-Assembly (EISA method using titanium isopropoxide and a cationic surfactant. The titania phase could be tuned by simply varying the aging time. As the aging time increased, hierarchically structured mesoporous materials with mixed phases of titania were obtained. The rutile content was found to generally increase with length in aging time. The mesostructured materials were evaluated for hydrogen production, and a mixed phase consisting of 95% anatase and 5% rutile showed the highest activity. This study indicates that the aging time is an important parameter for the preparation of mesostructured materials with hierarchical porosities and mixed phase(s of titania.

  6. Solid-phase microextraction: a promising technique for sample preparation in environmental analysis.

    Science.gov (United States)

    Alpendurada, M F

    2000-08-11

    Solid-phase microextraction (SPME) is a simple and effective adsorption and desorption technique, which eliminates the need for solvents or complicated apparatus, for concentrating volatile or nonvolatile compounds in liquid samples or headspace. SPME is compatible with analyte separation and detection by gas chromatography and high-performance liquid chromatography, and provides linear results for wide concentrations of analytes. By controlling the polarity and thickness of the coating on the fibre, maintaining consistent sampling time, and adjusting other extraction parameters, an analyst can ensure highly consistent, quantifiable results for low concentration analytes. To date, about 400 articles on SPME have been published in different fields, including environment (water, soil, air), food, natural products, pharmaceuticals, biology, toxicology, forensics and theory. As the scope of SPME grew, new improvements were made with the appearance of new coatings that allowed an increase in the specificity of this extraction technique. The key part of the SPME fibre is of course the fibre coating. At the moment, 27 variations of fibre coating and size are available. Among the newest are a fibre assembly with a dual coating of divinylbenzene and Carboxen suspended in poly(dimethylsiloxane), and a series of 23 gauge fibres intended for specific septumless injection system. The growth of SPME is also reflected in the expanding number of the accessories that make the technology even easier to use Also available is a portable field sampler which is a self-contained unit that stores the SPME fibre after sampling and during the shipment to the laboratory. Several scientific publications show the results obtained in inter-laboratory validation studies in which SPME was applied to determine the presence of different organic compounds at ppt levels, which demonstrates the reliability of this extraction technique for quantitative analysis.

  7. Preparation of porous microsphere-scaffolds by electrohydrodynamic forming and thermally induced phase separation

    Energy Technology Data Exchange (ETDEWEB)

    Ghanbar, Hanif; Luo, C.J.; Bakhshi, Poonam [Department of Mechanical Engineering, University College London, Torrington Place, London, WC1E 7JE (United Kingdom); Day, Richard [Division of Medicine, University College London, Rockefeller Building, 21 University Street, London, WC1E 6JJ (United Kingdom); Edirisinghe, Mohan, E-mail: m.edirisinghe@ucl.ac.uk [Department of Mechanical Engineering, University College London, Torrington Place, London, WC1E 7JE (United Kingdom)

    2013-07-01

    The availability of forming technologies able to mass produce porous polymeric microspheres with diameters ranging from 150 to 300 μm is significant for some biomedical applications where tissue augmentation is required. Moreover, appropriate assembly of microspheres into scaffolds is an important challenge to enable direct usage of the as-formed structures in treatments. This work reports the production of poly (glycolic-co-lactic acid) and poly (ε-caprolactone) microspheres under ambient conditions using one-step electrohydrodynamic jetting (traditionally known as atomisation) and thermally induced phase separation (TIPS). To ensure robust production for practical uses, this work presents 12 comprehensive parametric mode mappings of the diameter distribution profiles of the microspheres obtained over a broad range of key processing parameters and correlating of this with the material parameters of 5 different polymer solutions of various concentrations. Poly (glycolic-co-lactic acid) (PLGA) in Dimethyl carbonate (DMC), a low toxicity solvent with moderate conductivity and low dielectric constant, generated microspheres within the targeted diameter range of 150–300 μm. The fabrication of the microspheres suitable for formation of the scaffold structure is achieved by changing the collection method from distilled water to liquid nitrogen and lyophilisation in a freeze dryer. Highlights: ► EHDA is a unique method for production of the desired size of microspheres. ► Polymer solution properties are used to tailor the size distribution of spheres. ► Process control parameters (flow rate and applied voltage) are key in size control. ► Combination of EHDA with TIPS provides porous microspheres for assembly of scaffold.

  8. Preparation of zeolite ANA crystal from zeolite Y by in situ solid phase iso-structure transformation.

    Science.gov (United States)

    Wang, Yi; Li, Xuguang; Xue, Zhiyuan; Dai, Linsen; Xie, Songhai; Li, Quanzhi

    2010-05-06

    A new method has been explored to synthesize zeolite ANA crystals with regular icositetrahedron in aqueous media via transformation of zeolite Y under the conditions of low temperature, short reaction time, and without organic template. The products are perfect, almost 100% crystals. The samples prepared at different crystallization stages are measured by XRD, TEM, and SEM to investigate the transformation mechanism from zeolite Y to zeolite ANA. It has been demonstrated for the first time that the mechanism of forming a zeolite ANA polycrystal with sphere or shell morphologies is the in situ solid phase iso-structure transformation (Is-SPIST) of zeolite Y. The Is-SPIST mechanism is also supported by the results of steam-induced crystallization experiments and other assistant means, including the same Si/Al ratio, the same weight, the same particle size, and the same morphology before and after transformation of zeolite Y to zeolite ANA. It is also observed that a spherical or shell ANA polycrystal is constructed via the reconstruction from its exterior to interior, to form an ANA single crystal with a solid or hollow icositetrahedron. The main driving force of the reconstruction is considered to be the grain boundary energy existing between polycrystalline grains. This process also obeys the mechanism of in situ solid phase reconstruction (Is-SPR). Furthermore, the size and morphology of the zeolite ANA single crystal can be modified by surfactants.

  9. Preparation of electrospun Ag/TiO2 nanotubes with enhanced photocatalytic activity based on water/oil phase separation

    Science.gov (United States)

    Wang, Tao; Wei, Jinxin; Shi, Huimin; Zhou, Ming; Zhang, Yu; Chen, Qi; Zhang, Zhengmei

    2017-02-01

    Ag/TiO2 composite nanotubes were prepared by electrospinning based on water/oil phase separation effect, their photocatalytic abilities were evaluated under the UV-visible light irradiation. Comparing with bare TiO2 nanofibers, Ag/TiO2 nanotubes exhibited enhanced photocatalytic activities in the decomposition of Rhodamine B (RhB) solution. The enhanced photocatalytic activity of Ag/TiO2 nanotubes stems from the improved separation of photo-generated electron-hole pairs induced by Ag and the high dyes absorption ability of Ag/TiO2 nanotubes; the high specific surface areas of Ag/TiO2 nanotubes with large amounts of active sites, speeding the photocatalytic activity up; the short diffusion path of photo-generated carriers caused by thin thickness of Ag/TiO2 nanotubes. The strategy, fabrication electrospun Ag/TiO2 hybrid nanotubes based on water/oil phase separation effect, is a one step, simple and versatile method, which can be easily expanded to the fabrication of other materials for photocatalysis, water splitting and energy conversion.

  10. DETERMINATION OF FLUORIDE IN HIGHLY SALINATED WATERS BY ION CHROMATOGRAPHY METHOD WITH USE OF SOLID PHASE EXTRACTION FOR SAMPLE PREPARATION

    Directory of Open Access Journals (Sweden)

    Beata Kostka

    2014-10-01

    Full Text Available Solid phase extraction (SPE is one of the most popular methods of matrix elimination in determination of anions by ion chromatography. Possibility of using cartridges containing a cation-exchange resin in the Ag+ and Na+ forms for determination of fluoride in the presence of very high concentration of chloride in mine waters was described in this paper. A Dionex ICS-2500 ion chromatograph was used for separation of anions in gradient elution using IonPac AS19 (4x250 mm separation column along with generated KOH eluent. Fluoride after separation was determined by conductivity detector with suppression. The investigations performed on mine waters (conductivity in the range 12 700 μS/cm–155 000 μS/cm and synthetic brine (38 820 mg/L Cl- and 3 408 mg/L SO4 2- confirmed usefulness of cartridges containing a cation-exchange resin for minimizing matrix influence on results of fluoride determination. The ion chromatography method accompanied by solid phase extraction for sample preparation proved to be very useful for determination of fluoride in highly salinated waters (i.e. mine waters because of low detection limit (0,02 mg/L, good precision (< 2,5 % and accuracy (recovery 91 % – 104 %.

  11. Preparation of polydopamine-coated magnetic nanoparticles for dispersive solid-phase extraction of water-soluble synthetic colorants in beverage samples with HPLC analysis.

    Science.gov (United States)

    Chai, Weibo; Wang, Huijuan; Zhang, Ying; Ding, Guosheng

    2016-01-01

    A facile and sensitive dispersive solid-phase extraction (D-SPE) method for the extraction and enrichment of four representative synthetic colorants prior to high performance liquid chromatography analysis was introduced. As highly efficient adsorbents, polydopamine-coated Fe3O4 nanoparticles (Fe3O4@PDA NPs) were prepared by a simple and green procedure. Several factors affecting the extraction efficiency, mainly including the polymerization time of dopamine, pH of the sample solution, the amount of adsorbent, extraction time and the desorption conditions, were systematically studied. Under the optimized conditions, the enrichment factors for the four colorants were both higher than 176. The limits of detection (LODs) for the established d-SPE-HPLC method were found to be 0.20-0.25μgL(-1), which were lower than most chromatographic methods previously reported for synthetic colorant analysis. When used for quantitative analysis, wide linearity ranges (1-500μgL(-1) for amaranth and Ponceau 4R, and 0.80-500μgL(-1) for sunset yellow and allure red) were achieved with good correlation (R(2)≥0.9995). The developed method was also successfully applied to the analysis of colorants in beverage samples with satisfactory results, demonstrating its reliability and feasibility in real sample analysis.

  12. Preparation of magnetite-loaded silica microspheres for solid-phase extraction of genomic DNA from soy-based foodstuffs.

    Science.gov (United States)

    Shi, Ruobing; Wang, Yucong; Hu, Yunli; Chen, Lei; Wan, Qian-Hong

    2009-09-04

    Solid-phase extraction has been widely employed for the preparation of DNA templates for polymerase chain reaction (PCR)-based analytical methods. Among the variety of adsorbents studied, magnetically responsive silica particles are particularly attractive due to their potential to simplify, expedite, and automate the extraction process. Here we report a facile method for the preparation of such magnetic particles, which entails impregnation of porous silica microspheres with iron salts, followed by calcination and reduction treatments. The samples were characterized using powder X-ray diffractometry (XRD), scanning electron microscopy (SEM), nitrogen adsorption/desorption isotherms, and vibrating sample magnetometry (VSM). XRD data show that magnetite nanocrystals of about 27.2 nm are produced within the pore channels of the silica support after reduction. SEM images show that the as-synthesized particles exhibit spherical shape and uniform particle size of about 3 microm as determined by the silica support. Nitrogen sorption data confirm that the magnetite-loaded silica particles possess typical mesopore structure with BET surface area of about 183 m(2)/g. VSM data show that the particles display paramagnetic behavior with saturation magnetization of 11.37 emu/g. The magnetic silica microspheres coated with silica shells were tested as adsorbents for rapid extraction of genomic DNA from soybean-derived products. The purified DNA templates were amplified by PCR for screening of genetically modified organisms (GMOs). The preliminary results confirm that the DNA extraction protocols using magnetite-loaded silica microspheres are capable of producing DNA templates which are inhibitor-free and ready for downstream analysis.

  13. On the solid phase crystallization of In2O3:H transparent conductive oxide films prepared by atomic layer deposition

    Science.gov (United States)

    Macco, Bart; Verheijen, Marcel A.; Black, Lachlan E.; Barcones, Beatriz; Melskens, J.; Kessels, Wilhelmus M. M.

    2016-08-01

    Hydrogen-doped indium oxide (In2O3:H) has emerged as a highly transparent and conductive oxide, finding its application in a multitude of optoelectronic devices. Recently, we have reported on an atomic layer deposition (ALD) process to prepare high quality In2O3:H. This process consists of ALD of In2O3:H films at 100 °C, followed by a solid phase crystallization step at 150-200 °C. In this work, we report on a detailed electron microscopy study of this crystallization process which reveals new insights into the crucial aspects for achieving the large grain size and associated excellent properties of the material. The key finding is that the best optoelectronic properties are obtained by preparing the films at the lowest possible temperature prior to post-deposition annealing. Electron microscopy imaging shows that such films are mostly amorphous, but feature a very low density of embedded crystallites. Upon post-deposition annealing, crystallization proceeds merely from isotropic crystal grain growth of these embedded crystallites rather than by the formation of additional crystallites. The relatively high hydrogen content of 4.2 at. % in these films is thought to cause the absence of additional nucleation, thereby rendering the final grain size and optoelectronic properties solely dependent on the density of embedded crystallites. The temperature-dependent grain growth rate has been determined, from which an activation energy of (1.39 ± 0.04) eV has been extracted. Finally, on the basis of the observed crystallization mechanism, a simple model to fully describe the crystallization process has been developed. This model has been validated with a numerical implementation thereof, which accurately predicts the observed temperature-dependent crystallization behaviour.

  14. Preparation of metal wire supported solid-phase microextraction fiber coated with multi-walled carbon nanotubes.

    Science.gov (United States)

    Feng, Juanjuan; Sun, Min; Xu, Lili; Li, Jubai; Liu, Xia; Jiang, Shengxiang

    2011-09-01

    Multi-walled carbon nanotubes-coated solid-phase microextraction fiber was prepared by a novel protocol involving mussel-adhesive-protein-inspired polydopamine film. The polydopamine was used as binding agent to immobilize amine-functionalized multi-walled carbon nanotubes onto the surface of the stainless steel wire via Michael addition or Schiff base reaction. Surface properties of the fiber were characterized by field emission scanning electron microscope and X-ray photoelectron spectroscope. Six phenols in aqueous solution were used as model compounds to investigate the extraction performance of the fiber and satisfactory results were obtained. Limit of detection was 0.10 μg/L for 2-methylphenol (2-MP) and 4-methylphenol (4-MP), and 0.02 μg/L for 2-ethylphenol (2-EP), 4-ethylphenol (4-EP), 2-tert-butylphenol (2-t-BuP), and 4-tert-butylphenol (4-t-BuP), which were much lower than commercial fiber and fibers made in laboratory. RSDs for one unique fiber are in the range of 1.92-7.00%. Fiber-to-fiber (n=3) reproducibility ranges from 4.44 to 8.41%. It also showed very high stability and durability to acid, alkali, organic solvent, and high temperature. Real water sample from Yellow river was applied to test the reliability of the established solid-phase microextraction (SPME)-GC method and recoveries with addition level at 5 and 100 μg/L were in the range from 81.5 to 110.0%.

  15. Preparation and Thermal Stability of Ultrafine Nickel Powders Containing hcp-Ni Nanocrystallites Using Liquid-Phase Reduction Method

    Science.gov (United States)

    Xia, Zhimei; Jin, Shengming; Liu, Kun

    2016-10-01

    Ultrafine nickel powders containing hexagonal close-packed nickel (hcp-Ni) nanocrystallites were prepared using liquid-phase reduction with NiC2O4, NaOH, polyvinylpyrrolidone (PVP), and ethylene glycol (EG). The nickel powders were characterized by XRD and SEM. TG analysis was used to determine the thermal stability of ultrafine nickel powders. The results showed that nickel powders with 45.1 pct of hcp-Ni nanocrystallites were synthesized under the following conditions: a reflux time of 3 hours, an NiC2O4-to-EG molar ratio of 0.01, 5 g/L PVP, and 85 g/L NaOH. SEM results illustrated that spherical particles of size 500 nm were obtained. The results of thermal stability showed that the antioxidant property at high temperature was improved with the increase of hcp-Ni content. The oxidation rate of nickel powders with 43.3 pct hcp-Ni was less than 50 pct even if the temperature was up to 873 K (600 °C).

  16. Preparation and adsorption performance of 5-azacytosine-functionalized hydrothermal carbon for selective solid-phase extraction of uranium.

    Science.gov (United States)

    Song, Qiang; Ma, Lijian; Liu, Jun; Bai, Chiyao; Geng, Junxia; Wang, Hang; Li, Bo; Wang, Liyue; Li, Shoujian

    2012-11-15

    A new solid-phase extraction adsorbent was prepared by employing a two-step "grafting from" approach to anchor a multidentate N-donor ligand, 5-azacytosine onto hydrothermal carbon (HTC) microspheres for highly selective separation of U(VI) from multi-ion system. Fourier-transform infrared and X-ray photoelectron spectroscopies were used to analyze the chemical structure and properties of resultant HTC-based materials. The adsorption behavior of U(VI) onto the adsorbent was investigated as functions of pH, contact time, ionic strength, temperature, and initial U(VI) concentration using batch adsorption experiments. The U(VI) adsorption was of pH dependent. The adsorption achieved equilibrium within 30 min and followed a pseudo-second-order equation. The adsorption amount of U(VI) increased with raising the temperature from 283.15 to 333.15K. Remarkably, high ionic strength up to 5.0 mol L(-1) NaNO(3) had only slight effect on the adsorption. The maximum U(VI) adsorption capacity reached 408.36 mg g(-1) at 333.15K and pH 4.5. Results from batch experiments in a simulated nuclear industrial effluent, containing 13 co-existing cations including uranyl ion, showed a high adsorption capacity and selectivity of the adsorbent for uranium (0.63 mmol U g(-1), accounting for about 67% of the total adsorption amount).

  17. Preparation and characterization of porous DVB copolymers and their applicability for adsorption (solid-phase extraction) of phenol compounds

    Science.gov (United States)

    Sobiesiak, Magdalena; Podkoscielna, Beata

    2010-12-01

    Using DVB, three new porous copolymers in the form of microspheres were prepared, characterized and used as adsorbents for phenol and its chlorinated derivatives. As the monomers: 4,4'-bis(maleimidodiphenyl)methane (BM), 2,3-bis(2-hydroxy-3-methylacryloyloxy-propoxy)naphthalene (2,3-NAF) and 2,3-epoxypropyl methacrylate (GLY) were used. All the studied materials were synthesized under the same conditions by means of suspension copolymerization. The DVB copolymers were characterized by elemental analysis, FTIR spectroscopy, TG and DSC analyses and N 2 sorption. The off-line solid-phase extraction method (SPE) was used to estimate sorption properties of the copolymers. The results show that the newly obtained materials are mesoporous but their shape of pores and chemical structures are different. BM-DVB and GLY-DVB are characterized by slit-shaped pores and wide pore size distribution. 2,3-NAF-DVB also possesses slit pores but distribution of pore size is narrower. Of those studied BM-DVB is the most interesting material. It has good sorption properties and heat resistance.

  18. Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong

    2013-07-01

    A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column.

  19. Liquid-solid sample preparation followed by headspace solid-phase microextraction determination of multiclass pesticides in soil.

    Science.gov (United States)

    Durović, Rada D; Dordević, Tijana M; Santrić, Ljiljana R

    2012-01-01

    This paper describes development and validation of a multiresidue method for the determination of five pesticides (terbufos, prochloraz, chloridazon, pendimethalin, and fluorochloridone) belonging to different pesticide groups in soil samples by GC/MS, followed by its application in the analysis of some agricultural soil samples. The method is based on a headspace solid-phase microextraction method. Microextraction conditions, namely temperature, extraction time, and NaCI content, were tested and optimized using a 100 microm polydimethylsiloxane fiber. Three extraction solvents [methanol, methanol-acetone (1 + 1, v/v), and methanol-acetone-hexane (2 + 2 + 1, v/v/v)] and the optimum number of extraction steps within the sample preparation stage were optimized for the extraction procedure. LOD values for all the studied compounds were less than 12 microg/kg. Recovery values for multiple analyses of soil samples fortified at 30 microg/kg of each pesticide were higher than 64%. The method was proven to be repeatable, with RSD lower than 15%.

  20. High-Efficiency Photovoltaic Devices using Trap-Controlled Quantum-Dot Ink prepared via Phase-Transfer Exchange.

    Science.gov (United States)

    Aqoma, Havid; Al Mubarok, Muhibullah; Hadmojo, Wisnu Tantyo; Lee, Eun-Hye; Kim, Tae-Wook; Ahn, Tae Kyu; Oh, Seung-Hwan; Jang, Sung-Yeon

    2017-05-01

    Colloidal-quantum-dot (CQD) photovoltaic devices are promising candidates for low-cost power sources owing to their low-temperature solution processability and bandgap tunability. A power conversion efficiency (PCE) of >10% is achieved for these devices; however, there are several remaining obstacles to their commercialization, including their high energy loss due to surface trap states and the complexity of the multiple-step CQD-layer-deposition process. Herein, high-efficiency photovoltaic devices prepared with CQD-ink using a phase-transfer-exchange (PTE) method are reported. Using CQD-ink, the fabrication of active layers by single-step coating and the suppression of surface trap states are achieved simultaneously. The CQD-ink photovoltaic devices achieve much higher PCEs (10.15% with a certified PCE of 9.61%) than the control devices (7.85%) owing to improved charge drift and diffusion. Notably, the CQD-ink devices show much lower energy loss than other reported high-efficiency CQD devices. This result reveals that the PTE method is an effective strategy for controlling trap states in CQDs. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Dummy molecularly imprinted mesoporous silica prepared by hybrid imprinting method for solid-phase extraction of bisphenol A.

    Science.gov (United States)

    Yu, Dan; Hu, Xiaolei; Wei, Shoutai; Wang, Qiang; He, Chiyang; Liu, Shaorong

    2015-05-29

    A novel hybrid dummy imprinting strategy was developed to prepare a mesoporous silica for the solid-phase extraction (SPE) of bisphenol A (BPA). A new covalent template-monomer complex (BPAF-Si) was first synthesized with 2,2-bis(4-hydroxyphenyl)hexafluoropropane (BPAF) as the template. The imprinted silica was obtained through the gelation of BPAF-Si with tetraethoxysilane and the subsequent removal of template by thermal cleavage, and then it was characterized by FT-IR spectroscopy, scanning electron microscopy, transmission electron microscopy, and nitrogen adsorption-desorption isotherms. Results showed that the new silica had micron-level particle size and ordered mesoporous structure. The static binding test verified that the imprinted silica had much higher recognition ability for BPA than the non-imprinted silica. The imprinted silica also showed high extraction efficiencies and high enrichment factor for SPE of BPA. Using the imprinted silica, a SPE-HPLC-UV method was developed and successfully applied for detecting BPA in BPA-spiked tap water and lake water samples with a recovery of 99-105%, a RSD of 2.7-5.0% and a limit of detection (S/N=3) of 0.3ng/mL. The new imprinted silica avoided the interference of the residual template molecules and reduced the non-specific binding sites, and therefore it can be utilized as a good sorbent for SPE of BPA in environmental water samples.

  2. Preparation and electrochemical characterization of PPy-LiFePO{sub 4}/C composites via vapor-phase polymerization

    Energy Technology Data Exchange (ETDEWEB)

    Gong, Q.; Liao, X.Z.; He, Y.; Yang, Y.; Ma, Z.F. [Shanghai Jiao Tong Univ. (China). Dept. of Chemical Engineering

    2010-07-01

    Polypyrrole (PPy) is now being used as a means of improving the electrochemical performance of lithium-iron (LiFePO{sub 4}/C) composite electrode materials for Li-ion batteries. In this study, core-shell LiFePO{sub 4}/C-PPy composites were prepared using a chemical vapor-phase polymerization technique. Transmission electron microscopy (TEM) analyses demonstrated that the LiFePO{sub 4}/C particles were encapsulated with 7.5-nm thick PPy shells. Electrochemical analyses indicated that the high rate capacities and cycle stability of the composite materials was improved when compared with the performance of LiFePO{sub 4}/C composites. Tests on an MCMB/LiFePO{sub 4}-PPy fuel cell showed that the PPy coating reduced Fe dissolution from the LiFePO{sub 4} cathode, and alleviated subsequent Fe deposition on the MCMB anode, thereby enhancing the cell's life cycle. 7 refs., 2 figs.

  3. The ortho backbone amide linker (o-BAL) is an easily prepared and highly acid-labile handle for solid-phase synthesis

    DEFF Research Database (Denmark)

    Boas, Ulrik; Brask, Jesper; Christensen, J.B.;

    2002-01-01

    The tris(alkoxy)benzyl backbone amide linker (BAL) has found widespread application in solid-phase synthesis. The key intermediate for preparation of para BAL (p-BAL) is 2,6-dimethoxy-4-hydroxybenzaldehyde; several reports on its synthesis have appeared. However, the ortho analogue of the handle (o...

  4. Preparing different phases of Mg-Li-Sm alloys by molten salt electrolysis in LiCl-KCl-MgCl_2-SmCl_3 melts

    Institute of Scientific and Technical Information of China (English)

    韩伟; 田阳; 张密林; 叶克; 赵全友; 魏树权

    2010-01-01

    Different phases of Mg-Li-Sm alloys were prepared by galvanostatic electrolysis in LiCl-KCl-MgCl2-SmCl3 melts at 670 °C.The electrolysis process and phase control of Mg-Li-Sm alloys were studied.The microstructures of α,α+β,β phases of Mg-Li-Sm alloys were characterized by X-ray diffraction(XRD) and optical microscope(OM).Analysis of scanning electron microscopy(SEM) and EDS mapping analysis showed that Mg distributed homogeneously in Mg-Li-Sm alloys.EDS result showed that the distribution of Sm was more at...

  5. Isolation and Purification of Unstable Iridoid Glucosides from Traditional Chinese Medicine by Preparative High Performance Liquid Chromatography Coupled with Solid-phase Extraction

    Institute of Scientific and Technical Information of China (English)

    LI Cun-man; XIAO Yuan-sheng; XUE Xing-ya; FENG Jia-tao; ZHANG Xiu-li; LIANG Xin-miao

    2011-01-01

    An efficient preparative method was successfully developed for isolation and purification of unstable components from medicinal plant extracts, using a combined method of preparative high performance liquid chro matography(HPLC) and solid-phase extraction(SPE). The aim of this study was to obtain an effective method with high preparative efficiency and importantly to avoid the transformation of unstable compounds. The preparative HPLC system was based on an LC/MS controlled four-channel autopurification system. The SPE method was per formed with a C1s packing material to trap the target compounds and to remove the acidic additive derived from the mobile phase. Using this method, the unstable iridoid glucosides(IGs) as model compounds were successfully iso lated and purified from the extract of Hedyotis diffusa Willd. Six IGs(including one new minor IG) and one nucleo tide compound were simultaneously obtained, each with a purity of >91% as determined by HPLC. The structures of the isolated compounds were identified by UPLC/Q-TOF MS, UV, ID and/or 2D NMR. It was demonstrated that the combination of preparative HPLC with SPE is a versatile tool for preparative purification of unstable compounds from complex natural products.

  6. Isolation and Purification of Unstable Iridoid Glucosides from Traditional Chinese Medicine by Preparative High Performance Liquid Chromatography Coupled with Solid-phase Extraction

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    An efficient preparative method was successfully developed for isolation and purification of unstable components from medicinal plant extracts, using a combined method of preparative high performance liquid chro-matography(HPLC) and solid-phase extraction(SPE). The aim of this study was to obtain an effective method with high preparative efficiency and importantly to avoid the transformation of unstable compounds. The preparative HPLC system was based on an LC/MS controlled four-channel autopurification system. The SPE method was performed with a C18 packing material to trap the target compounds and to remove the acidic additive derived from the mobile phase. Using this method, the unstable iridoid glucosides(IGs) as model compounds were successfully isolated and purified from the extract of Hedyotis diffusa Willd. Six IGs(including one new minor IG) and one nucleotide compound were simultaneously obtained, each with a purity of 〉91% as determined by HPLC. The structures of the isolated compounds were identified by UPLC/Q-TOF MS, UV, 1D and/or 2D NMR. It was demonstrated that the combination of preparative HPLC with SPE is a versatile tool for preparative purification of unstable compounds from complex natural products.

  7. Charge-discharge studies on a lithium cell composed of PVdF-HFP polymer membranes prepared by phase inversion technique with a nanocomposite cathode

    Science.gov (United States)

    Manuel Stephan, A.; Teeters, Dale

    A novel polymer membrane of poly(vinylidene fluoride-hexafluoropropylene) (PVdF-HFP) co-polymer was prepared by the phase inversion technique with two different non-solvents, 1-butanol or hexane. The prepared films were analyzed by scanning electron microscope (SEM) and nitrogen absorption/desorption techniques. The change in the morphology and pore diameter of the films prepared with different non-solvents correlates with the structure of the non-solvents used. This electrolyte membrane was coupled with a nanocomposite LiAl 0.01Co 0.99O 2 cathode which was prepared by a solid-state reaction method and subsequently by ball-milling. Lithium cells consisting of LiAl 0.01Co 0.99O 2/polymer electrolyte/Li were assembled and their charge-discharge studies were investigated.

  8. Effects of Ni doping on photocatalytic activity of TiO2 thin films prepared by liquid phase deposition technique

    Indian Academy of Sciences (India)

    Noor Shahina Begum; H M Farveez Ahmed; K R Gunashekar

    2008-10-01

    The TiO2 thin films doped by Ni uniformly and non-uniformly were prepared on glass substrate from an aqueous solution of ammonium hexa-fluoro titanate and NiF2 by liquid phase deposition technique. The addition of boric acid as an – scavenger will shift the equilibrium to one side and thereby deposition of the film is progressed. The rate of the reaction and the nature of deposition depend on growing time and temperature. The resultant films were characterized by XRD, EDAX, UV and SEM. The result shows that the deposited films have amorphous background, which becomes crystalline at 500°C. The EDAX data confirms the existence of Ni atoms in TiO2 matrix. XRD analysis reveals the peaks corresponding to Ni but no peak of crystalline NiO was found. The transmittance spectra of Ni uniformly and non-uniformly doped TiO2 thin films show `blue shift and red shift’, respectively. Ni-doped TiO2 thin films can be used as photocatalyst for the photodegradation of methyl orange dye. It was found that, organic dye undergoes degradation efficiently in presence of non-uniformly Ni-doped TiO2 thin films when compared to uniformly doped films and pure TiO2 films under visible light. The photocatalytic activity increases with increase in the concentration of Ni in case of nonuniformly doped thin films but decreases with the concentration when uniformly doped thin films were used.

  9. A novel polythiophene – ionic liquid modified clay composite solid phase microextraction fiber: Preparation, characterization and application to pesticide analysis

    Energy Technology Data Exchange (ETDEWEB)

    Pelit, Füsun Okçu, E-mail: fusun.okcu@ege.edu.tr; Pelit, Levent; Dizdaş, Tuğberk Nail; Aftafa, Can; Ertaş, Hasan; Yalçınkaya, E.E.; Türkmen, Hayati; Ertaş, F.N.

    2015-02-15

    Highlights: • A novel polythiophene – ionic liquid modified clay surface has been prepared. • Polymerization was performed electrochemically on a stainless steel wire. • This material was used as a SPME fiber in head space mode. • This new SPME fiber was applied for analysis of pesticides in juice samples. • Fiber adsorption properties were improved by modification of ionic liquids. - Abstract: This report comprises the novel usage of polythiophene – ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett–Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box–Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002–0.667 ng mL{sup −1}. Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues.

  10. Electron Scattering and Doping Mechanisms in Solid-Phase-Crystallized In2O3:H Prepared by Atomic Layer Deposition.

    Science.gov (United States)

    Macco, Bart; Knoops, Harm C M; Kessels, Wilhelmus M M

    2015-08-01

    Hydrogen-doped indium oxide (In2O3:H) has recently emerged as an enabling transparent conductive oxide for solar cells, in particular for silicon heterojunction solar cells because its high electron mobility (>100 cm(2)/(V s)) allows for a simultaneously high electrical conductivity and optical transparency. Here, we report on high-quality In2O3:H prepared by a low-temperature atomic layer deposition (ALD) process and present insights into the doping mechanism and the electron scattering processes that limit the carrier mobility in such films. The process consists of ALD of amorphous In2O3:H at 100 °C and subsequent solid-phase crystallization at 150-200 °C to obtain large-grained polycrystalline In2O3:H films. The changes in optoelectronic properties upon crystallization have been monitored both electrically by Hall measurements and optically by analysis of the Drude response. After crystallization, an excellent carrier mobility of 128 ± 4 cm(2)/(V s) can be obtained at a carrier density of 1.8 × 10(20) cm(-3), irrespective of the annealing temperature. Temperature-dependent Hall measurements have revealed that electron scattering is dominated by unavoidable phonon and ionized impurity scattering from singly charged H-donors. Extrinsic defect scattering related to material quality such as grain boundary and neutral impurity scattering was found to be negligible in crystallized films indicating that the carrier mobility is maximized. Furthermore, by comparison of the absolute H-concentration and the carrier density in crystallized films, it is deduced that <4% of the incorporated H is an active dopant in crystallized films. Therefore, it can be concluded that inactive H atoms do not (significantly) contribute to defect scattering, which potentially explains why In2O3:H films are capable of achieving a much higher carrier mobility than conventional In2O3:Sn (ITO).

  11. Preparation of a silica stationary phase co-functionalized with Wulff-type phenylboronate and C12 for mixed-mode liquid chromatography.

    Science.gov (United States)

    Li, Hengye; Zhang, Xuemeng; Zhang, Lin; Wang, Xiaojin; Kong, Fenying; Fan, Dahe; Li, Lei; Wang, Wei

    2017-04-15

    A silica stationary phase was designed and synthesized through the co-functionalization of silica with Wulff-type phenylboronate and C12 for mixed-mode liquid chromatography applications. The as-synthesized stationary phase was characterized by elemental analysis and Fourier Transform-InfraRed Spectroscopy (FT-IR). Retention mechanisms, including boronate affinity (BA), reversed-phase (RP) and anion-exchange (AE), were involved. Retention mechanism switching was easily realized by adjustment of the mobile phase constitution. Cis-diol compounds could be selectively captured under neutral conditions in BA mode and off-line separated in RP mode. Neutral, basic, acidic and amphiprotic compounds were chromatographed on the column in RP chromatography, while inorganic anions were chromatographed in AE chromatography to characterize the mixed-mode nature of the prepared stationary phase. In addition, the RP performance was compared with an octadecyl silica column in terms of column efficiency (N/m), asymmetry factor (Af), retention factor (k) and resolution (Rs). The prepared stationary phase offered multiple interactions with analytes in addition to hydrophobic interactions under RP elution conditions. Based on the mixed-mode properties, off-line 2D-LC, for selective capture and separation of urinary nucleosides, was successfully realized on a single column, demonstrating its powerful application potential for complex samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Two-step preparation of nano-scaled magnetic chitosan particles using Triton X-100 reversed-phase water-in-oil microemulsion system

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Zhengkun; Jiang, Feihong [College of Food Science and Engineering, Northwest A and F University, Yangling, Shaanxi 712100 (China); Lee, Tung-Ching, E-mail: lee@aesop.rutgers.edu [Department of Food Science, Rutgers, the State University of New Jersey, 65 Dudley Road, New Brunswick, NJ 08901 (United States); Yue, Tianli, E-mail: yuetl305@nwsuaf.edu.cn [College of Food Science and Engineering, Northwest A and F University, Yangling, Shaanxi 712100 (China)

    2013-12-25

    Highlights: •A new two-step route for nano-scaled magnetic chitosan particles preparation. •Triton X-100 reversed-phase microemulsion system was used for chitosan coating. •Narrow size distribution of magnetic chitosan nanoparticles was achieved. •Quantitative evaluation of recoverability for the magnetic chitosan nanoparticles. -- Abstract: A new two-step route for the preparation of nano-scaled magnetic chitosan particles has been developed, different from reported one-step in situ preparation and two-step preparation method of reversed-phase suspension, Triton X-100 reversed-phase water-in-oil microemulsion encapsulation method was employed in coating the pre-prepared Fe{sub 3}O{sub 4} nanoparticles with chitosan. The resultant magnetic chitosan particles owned a narrow size distribution ranging from 50 to 92 nm. X-ray diffraction patterns (XRD) indicated that the chitosan coating procedure did not change the spinal structure of Fe{sub 3}O{sub 4} magnetic nanoparticles. The results of Fourier transform infrared (FTIR) analysis and thermogravimetric analysis (TGA) demonstrated that the chitosan was coated on Fe{sub 3}O{sub 4} nanoparticles and its average mass content was ∼50%. The saturated magnetization of the magnetic Fe{sub 3}O{sub 4}/chitosan nanoparticles reached 18.62 emu/g, meanwhile, the nanoparticles showed the characteristics of superparamagnetism. The magnetic chitosan nanoparticles showed a high recoverability of 99.99% in 10 min when pH exceeded 4. The results suggested that the as-prepared magnetic chitosan particles were nano-scaled with a narrow size distribution and a high recoverability.

  13. [Preparation and evaluation of 2,6-di-O-pentyl-beta-cyclodextrin bonded silica stationary phase for high performance liquid chromatography].

    Science.gov (United States)

    Liu, Liwen; Luo, Aiqin; Dai, Rongji; Ge, Xiaoxia; Yang, Shaoning

    2004-11-01

    In order to improve the chiral separation capability of the conventional beta-cyclodextrin bonded-silica gel stationary phase, 2,6-di-O-pentyl-beta-cyclodextrin bonded stationary phase (PCDS) was prepared via a long spacer. The resulted bonded-silica stationary phase was characterized by three methods, namely Fourier transform infrared, Molisch color reaction, X-ray optical electrical energy spectrogram. The chromatographic performances of PCDS were investigated by using liquid chromatography with toluene, dimethyl phthalate, and phenanthrene as solutes, and their retention mechanism was investigated and discussed. The results show that the introduction of pentyl to beta-cyclodextrin leads to enhancement of the retention of the solutes. The chiral separation capability of the new bonded-silica stationary phase was evaluated by using liquid chromatography with some chiral drugs. Some of the enantiomers such as chlorphenamine maleate and bupropion hydrochloride were separated by heptakis (2,6-di-O-pentyl)-beta-cyclodextrin bonded silica stationary.

  14. Optimizing Preparation of Micron SiO2-based Phase Change and Humidity Controlling Composites with Uniform Particle Size Distribution Based on RBF Neural Network

    Directory of Open Access Journals (Sweden)

    ZHANG Hao

    2017-08-01

    Full Text Available With SiO2 as the carrier, decanoic acid-palmitic acid as a phase change material,the micron SiO2-based phase change and humidity controlling composite materials were prepared by sol-gel method. The scheme was optimized by uniform design in a combination with RBF neural network to optimizing preparation of micron SiO2-based phase change and humidity controlling composite materials. The performance of micron SiO2-based phase change and humidity controlling composite materials with optimal uniform particle size distribution were tested and characterized. The results show that RBF neural network has the best approximation effect, when spread is 0.5; optimization technology parameters are solution pH value 4.27, amount of deionized water (mole ratio between deionized water and tetraethyl orthosilicate is 8.58, amount of absolute alcohol (mole ratio between absolute alcohol and tetraethyl orthosilicate is 4.83 and ultrasonic wave power is 316W; micron SiO2-based phase change and humidity controlling composite materials with optimal uniform particle size distribution' d10 is 383.51nm, d50 is 511.63nm and d90 is 658.76nm, measured value of d90-d10 is 275.25nm, the measured value and the predicted value are in good agreement (relative error is -2.64%; micron SiO2-based phase change and humidity controlling composite materials with optimal uniform particle size distribution' equilibrium moisture content in the relative humidity of 40%-60% is 0.0925-0.1493g/g, phase transition temperature is 20.02-23.45℃ and phase change enthalpy is 54.06-60.78J/g.

  15. COVALENTLY BONDING CHIRAL POLYURETHANE ON AMINATED SILICA GEL: A NEW STRATEGY TO PREPARE CHIRAL STATIONARY PHASE FOR HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

    Institute of Scientific and Technical Information of China (English)

    Shao-hua Huang; Zheng-wu Bai; Chuan-qi Yin; Shi-rong Li

    2006-01-01

    Two polyurethanes of different molecular weights were prepared by the copolymerization of phenyl diisocyanate and diisopropyl tartrate. The polyurethanes having terminal isocyanate groups were reacted with 3-aminopropyl silica gel to afford two chiral stationary phases. The (M-)n of the two polyurethanes were 4057 g/mol and 6442 g/mol. The polyurethanes and the corresponding chiral stationary phases were characterized by FT-IR, 1H NMR and elemental analysis. The loading capacities of the polyurethanes on silica gel were 0.68 mmol units/g and 0.61 mmol units/g, respectively. The separation performance and the influence of additives, triethylamine and trichloroacetic acid, on the separation of chiral compounds were investigated by HPLC. The chiral stationary phase prepared from polyurethane with (M-)n of 4057 g/mol demonstrated better enantioseparation capability than that with (M-)n of 6442 g/mol. Additionally, it was found that the addition of triethylamine and trichloroacetic acid in the mobile phases significantly improved the enantioseparation for these two chiral stationary phases.

  16. The Impact of Endurance Training on Functional Parameters During the Preparation Phase among Cross-Country Skiers

    Directory of Open Access Journals (Sweden)

    Žiška Peter

    2016-05-01

    Full Text Available In the study, we have tried to demonstrate the effect of endurance training on changes in functional parameters during the preparation phase (12-week mesocycle among cross-country skiers. The group consisted of 10 male cross-country skiers (age: 21.4 ±5 year who completed control (1st 6 week mesocycle and experimental period (2nd 6 week mesocycle.We focused on the following time-varying parameters: changes in maximal oxygen uptake (VO2max, the level of aerobic (AeT and anaerobic thresholds (AT, maximum heart rate (HRmax and performance on the running treadmill. The intra-individual monitoring of each athlete revealed statistical significance of VO2max (mid_VO2max = 69.48 ± 5.72 l.kg-1.min-1, post_ VO2max = 70.96 ± 5.67 ml.kg-1.min-1; p≤0.05 and the level of AT (mid_AT = 86.2 ± 5.43 %, post_AT = 87.8 ± 5.59 %; p≤0.01 the performance on the running treadmill (mid_t = 14:54 ± 1:43 min., post_t = 15:30 ± 1:50 min.; p≤0.05.The significant changes were recorded in the AeT(pre_AeT = 70.3 ± 7.56 %, mid_AeT = 72.5 ± 7.59 %; p≤0.05 in theHRmax(pre_HRmax = 190 ± 8.04 bpm, mid_HRmax = 189 bpm, post_HRmax = 188 ± 7.34 bpm; p = n.s. during control period. We assume that the significant differences occurred as a result of adaptation changes due to training stimuli, which were induced by changes in functional parameters. Increased training volume in zone lower level of oxygen regime (A1, upper level of oxygen regime (A2 and upper level of lactate tolerance(T2 during experimental period elicited changes which reflected the increase functional parameters and performance on the running treadmill compared to that of control period.

  17. Optimization of substrate preparation for oyster mushroom (Pleurotus ostreatus) cultivation by studying different raw materials and substrate preparation conditions (composting: phases I and II).

    Science.gov (United States)

    Vieira, Fabrício Rocha; de Andrade, Meire Cristina Nogueira

    2016-11-01

    In recent years, oyster mushroom (Pleurotus ostreatus) has become one of the most cultivated mushrooms in the world, mainly in Brazil. Among many factors involved in a mushroom production, substrate preparation is the most critical step, which can be influenced by composting management techniques. Looking forward to optimizing the substrate preparation process, were tested different composting conditions (7 and 14 days of composting with or without conditioning), potential raw materials (decumbens grass, brizantha grass and sugarcane straw) and nitrogen supplementation (with or without wheat bran) on oyster mushroom yield and biological efficiency (BE). The substrate composted for 7 days with conditioning showed higher yield and biological efficiency of mushroom (24.04 and 100.54 %, respectively). Substrates without conditioning (7 and 14 days of composting) showed smaller mushroom yield and biological efficiency. Among the raw materials tested, brizantha grass showed higher mushroom yield followed by decumbens grass, sugarcane straw and wheat straw (28.5, 24.32, 23.5 and 19.27 %, respectively). Brizantha grass also showed higher biological efficiency followed by sugarcane straw, decumbens grass and wheat straw (123.95, 103.70, 96.90 and 86.44 %, respectively). Supplementation with wheat bran improved yield and biological efficiency in all substrate formulations tested; thus, oyster mushroom yield and biological efficiency were influenced by substrate formulation (raw materials), supplementation and composting conditions.

  18. Influence of fuel on phase formation of ZnFe{sub 2}O{sub 4} prepared by self-propagated combustion route

    Energy Technology Data Exchange (ETDEWEB)

    Venkatesan, K.; Babu, D. Rajan, E-mail: drajanbabu@vit.ac.in [Advanced Materials Research Centre, Crystal Growth and Crystallography Division, School of Advanced Sciences, VIT University, Vellore – 632014 (India)

    2015-06-24

    Zinc iron oxide (ZnFe{sub 2}O{sub 4}) nanoparticles were prepared by self-propagated combustion route.The fuel plays a major role on the formation of structure and particle size. Here three different fuels like alanine, glycine and proline were used to synthesis the zinc iron oxide nanoparticle. Influence of combustion nature through the fuel, the phase formation, particle size, band gap and surface morphology has been modified. The prepared powder was characterized by powder X-ray diffraction method (PXRD), field-emission scanning electron microscopy (FE-SEM) and the composition of the material was analysed by X-ray energy dispersive spectroscopy (EDAX).The elemental mapping was confirmed the uniform distribution of Zn, Fe and O elements in the prepared material of ZnFe{sub 2}O{sub 4}.

  19. Preparation of Porous GaN Buffer and Its Influence on the Residual Stress of GaN Epilayers Grown by Hydride Vapor Phase Epitaxy

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    The preparation of porous structure on the molecular beam epitaxy (MBE)-grown mixed-polarity GaN epilayers was reported by using the wet chemical etching method. The effect of this porous structure on the residual stress of subsequent-growth GaN epilayers was studied by Raman and photoluminescence (PL) spectrum.Substantial decrease in the biaxial stresse can be achieved by employing the porous buffers in the hydride vapour phase epitaxy (HVPE) epilayer growth.

  20. LATTICE DEFORMATION AND PHASE TRANSFORMATION FROM NANO-SCALE ANATASE TO NANO-SCALE RUTILE TiO2 PREPARED BY A SOL-GEL TECHNIQUE

    Institute of Scientific and Technical Information of China (English)

    Yanqun Shao; Dian Tang; Jinghua Sun; Yekun Lee; Weihao Xiong

    2004-01-01

    Nano-scale rutile phase was transformed from nano-scale anatase upon heating, which was prepared by a sol-gel technique. The XRD data corresponding to the anatase and rutile phases were analyzed and the grain sizes of as-derived phases were calculated by Sherrer equation. The lattice parameters of the as-derived anatase and rutile unit cells were calculated and compared with those of standard lattice parameters on PDF cards. It was shown that the smaller the grain sizes, the larger the lattice deformation. The lattice parameter a has the negative deviation from the standard and the lattice parameter c has the positive deviation for both phases. The particles sizes had preferential influence on the longer parameter between the lattice parameters of a and c. With increasing temperatures, the lattice parameters of a and c in both phases approached to the equilibrium state. The larger lattice deformation facilitated the nucleation process, which lowered the transformation temperature. During the transformation from nano-scale anatase to rutile, besides the mechanism involving retention of the {112} pseudo-close-packed planes of oxygen in anatase as the{100} pseudo-close-packed planes in rutile, the new phase occurred by relaxation of lattice deformation and adjustment of the atomic sites in parent phase. The orientation relationships were suggested to be anatase {101}//rutile {101} and anatase //rutile, and the habit plane was anatase (101),

  1. Reclamation of acid pickling waste: A facile route for preparation of single-phase Fe{sub 3}O{sub 4} nanoparticle

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Wenxue; Lu, Bin; Tang, Huihui; Zhao, Jingxiang; Cai, Qinghai, E-mail: caiqinghai@yahoo.com

    2015-05-01

    Using an alternative method of dropwise addition of iron salt in NaOH aqueous solution, nanocrystalline Fe{sub 3}O{sub 4} materials were prepared from acid pickling waste as a starting material with ultrasonic enhancement and polyethylene glycol as a dispersant, as proved by XRD, TEM, TG–DSC and ICP-MS. The results showed that the Fe{sub 3}O{sub 4} material was a well-crystallized magnetite with an average size of about 25 nm and purity 99.15%. Magnetic measurement revealed the nanocrystals were stronger superparamagnetic with a saturation magnetization of 82.1 emu/g. - Graphical abstract: A facile method for the preparation of single-phase Fe{sub 3}O{sub 4} nanoparticle from acid pickling waste by chemical precipitation was explored. The results characterized by XRD, FT-IR, TEM, TG–DSC, ICP-MS and magnetic measurement showed that the obtained Fe{sub 3}O{sub 4} nanomaterial was well-crystallized magnetite and stronger superparamagnetic with single phase. - Highlights: • Reclamation of acid pickling waste. • An alternative route for preparation of Fe{sub 3}O{sub 4}. • Nanocrystals with single phase. • Stronger superparamagnetic nature.

  2. Separation of four flavonol glycosides from Solanum rostratum Dunal using aqueous two-phase flotation followed by preparative high-performance liquid chromatography.

    Science.gov (United States)

    Chang, Lin; Shao, Qian; Xi, Xingjun; Chu, Qiao; Wei, Yun

    2017-02-01

    Aqueous two-phase flotation followed by preparative high-performance liquid chromatography was used to separate four flavonol glycosides from Solanum rostratum Dunal. In the aqueous two-phase flotation section, the effects of sublation solvent, solution pH, (NH4 )2 SO4 concentration in aqueous solution, cosolvent, N2 flow rate, flotation time, and volumes of the polyethylene glycol phase on the recovery were investigated in detail, and the optimal conditions were selected: 50 wt% polyethylene glycol 1000 ethanol solvent as the flotation solvent, pH 4, 350 g/L of (NH4 )2 SO4 concentration in aqueous phase, 40 mL/min of N2 flow rate, 30 min of flotation time, 10.0 mL of flotation solvent volume, and two times. After aqueous two-phase flotation concentration, the flotation products were purified by preparative high-performance liquid chromatography. The purities of the final products A and B were 98.1 and 99.0%. Product B was the mixture of three compounds based on the analysis of high-performance liquid chromatography at the temperature of 10°C, while product A was hyperoside after the identification by nuclear magnetic resonance. Astragalin, 3'-O-methylquercetin 3-O-β-d-galactopyranoside, and 3'-O-methylquercetin 3-O-β-d-glucopyranoside were obtained with the purity of 93.8, 97.1, and 99.2%, respectively, after the further separation of product B using preparative high-performance liquid chromatography.

  3. PREPARATION OF MICROPOROUS ULTRA HIGH MOLECULAR WEIGHT POLYETHYLENE (UHMWPE) BY THERMALLY INDUCED PHASE SEPARATION OF A UHMWPE/LIQUID PARAFFIN MIXTURE

    Institute of Scientific and Technical Information of China (English)

    Lie Shen; Mao Peng; Fei Qiao; Jie-lai Zhang

    2008-01-01

    Ultra-high molecular weight polyethylene (UHMWPE) with a microporous structure was prepared via thermally induced phase separation (TIPS).Liquid paraffin (LP) was used as a diluent in the preparation of microporous UHMWPE.Small angle laser light scattering (SALLS) and differential scanning calorimetry (DSC) were used to determine the phase separation temperatures,I.e.the cloud points and the dynamic crystallization temperatures,respectively.It was found that the cloud points were coincident with the crystallization temperatures,indicating that a solid-liquid phase separation occurred during thermal quenching of the UHMWPE/LP solution,while,no liquid-liquid phase separation above the crystallization temperature was observed.The effects of the content and the molecular weight of UHMWPE on the morphology and average pore size were investigated with field emission scanning electron microscopy (FE-SEM) and mercury porosimetry.With the increase of the content of UHMWPE,the average pore size of the microporous material decreased and the molecular weight of UHMWPE could also influence the pore size slightly.

  4. Influence of cerium ions on the anatase-rutile phase transition of TiO2 prepared by sol-gel auto-igniting synthesis

    Institute of Scientific and Technical Information of China (English)

    YAN Qingzhi; SU Xintai; ZHOU Yanping; GE Changchun

    2005-01-01

    The anatase-rutile phase transformation of TiO2 doped cerium up to 5 mol% was studied by X-ray diffraction and X-ray photoelectron spectroscopy. The samples were prepared by sol-gel auto-igniting synthesis process from a TiO(NO3)2-Ce(NO3)2-NH4NO3-citric acid complex compound system. The combusted amorphous powders were calcined at different temperatures. Significant structural changes were observed during the various stages of the phase transformation.It was concluded that at low dopant contents, cerium ions were incorporated into the TiO2 structure, and the anatase phase was stabilized; but at larger amounts, part of the dopant was segregated on the surface of TiO2 and the rutile formation was accelerated at elevated calcination temperature.

  5. A Novel Route for Preparing Highly Stable Fe3O4 Fluid with Poly(Acrylic Acid) as Phase Transfer Ligand

    Science.gov (United States)

    Oanh, Vuong Thi Kim; Lam, Tran Dai; Thu, Vu Thi; Lu, Le Trong; Nam, Pham Hong; Tam, Le The; Manh, Do Hung; Phuc, Nguyen Xuan

    2016-08-01

    Highly stable Fe3O4 liquid was synthesized by thermal decomposition using poly(acrylic acid) (PAA) as a phase transfer ligand. The crystalline structure, morphology, and magnetic properties of the as-prepared samples were thoroughly characterized. Results demonstrated that the magnetic Fe3O4 nanomaterial was formed in liquid phase with a spinel single-phase structure, average size of 8-13 nm, and high saturation magnetization (up to 75 emu/g). The PAA-capped Fe3O4 nanoparticles displayed high stability over a wide pH range (from 4 to 7) in 300 mM salt solution. More importantly, the heat-generating capacity of the nanoparticle systems was quantified at a specific absorption rate (SAR) of 70.22 W/g, which is 35% higher than magnetic nanoparticles coated with sodium dodecyl sulfate (SDS). These findings suggest the potential application of PAA-coated magnetic nanoparticles in magnetic hyperthermia.

  6. Preparation of a hierarchically porous AlPO4 monolith via an epoxide-mediated sol–gel process accompanied by phase separation

    Directory of Open Access Journals (Sweden)

    Wenyan Li, Yang Zhu, Xingzhong Guo, Kazuki Nakanishi, Kazuyoshi Kanamori and Hui Yang

    2013-01-01

    Full Text Available Monolithic aluminum phosphate (AlPO4 with a macro–mesoporous structure has been successfully prepared via the sol–gel process accompanied by phase separation in the presence of poly(ethylene oxide (PEO. Gelation of the system has been mediated by propylene oxide (PO, while PEO induces a phase separation. The dried gel is amorphous, whereas the crystalline tridymite phase precipitates upon heating above 1000 °C. Heat treatment does not spoil the macroporous morphology of the AlPO4 monoliths. Nitrogen adsorption–desorption measurements revealed that the skeletons of the dried gels possess a mesostructure with a median pore size of about 30 nm and a surface area as high as 120 m2 g−1. Hydrothermal treatment before heat treatment can increase the surface area to 282 m2 g−1.

  7. Preparation of a hierarchically porous AlPO4 monolith via an epoxide-mediated sol-gel process accompanied by phase separation

    Science.gov (United States)

    Li, Wenyan; Zhu, Yang; Guo, Xingzhong; Nakanishi, Kazuki; Kanamori, Kazuyoshi; Yang, Hui

    2013-08-01

    Monolithic aluminum phosphate (AlPO4) with a macro-mesoporous structure has been successfully prepared via the sol-gel process accompanied by phase separation in the presence of poly(ethylene oxide) (PEO). Gelation of the system has been mediated by propylene oxide (PO), while PEO induces a phase separation. The dried gel is amorphous, whereas the crystalline tridymite phase precipitates upon heating above 1000 °C. Heat treatment does not spoil the macroporous morphology of the AlPO4 monoliths. Nitrogen adsorption-desorption measurements revealed that the skeletons of the dried gels possess a mesostructure with a median pore size of about 30 nm and a surface area as high as 120 m2 g-1. Hydrothermal treatment before heat treatment can increase the surface area to 282 m2 g-1.

  8. Preparation and thermal characterization of oxalic acid dihydrate/bentonite composite as shape-stabilized phase change materials for thermal energy storage

    Science.gov (United States)

    Han, Lipeng; Xie, Shaolei; Sun, Jinhe; Jia, Yongzhong

    2017-03-01

    Oxalic acid dihydrate (OAD) which has very high initial phase transition enthalpy is a promising phase change material (PCM). In this paper, shape-stabilized composite PCMs composed of OAD and bentonite were prepared by a facile blending method to overcome the problem of leakage. FT-IR results indicated the interactions between OAD and bentonite, such as the capillary force and the hydrogen bonding, resulting in the confined crystallization process. As a result, the OAD was confined to be amorphous. The thermogravimetric analysis and scanning electron microscope results showed that sample had the best coating effect when the amount of bentonite was 17.7%. The differential scanning calorimetry analyses demonstrated that a decrease in the OAD content was accompanied by a continuous decrease in the melting point and phase change enthalpy of the composites.

  9. Releasing intracellular product to prepare whole cell biocatalyst for biosynthesis of Monascus pigments in water-edible oil two-phase system.

    Science.gov (United States)

    Hu, Minglue; Zhang, Xuehong; Wang, Zhilong

    2016-11-01

    Selective releasing intracellular product in Triton X-100 micelle aqueous solution to prepare whole cell biocatalyst is a novel strategy for biosynthesis of Monascus pigments, in which cell suspension culture exhibits some advantages comparing with the corresponding growing cell submerged culture. In the present work, the nonionic surfactant Triton X-100 was successfully replaced by edible plant oils for releasing intracellular Monascus pigments. High concentration of Monascus pigments (with absorbance nearly 710 AU at 470 nm in the oil phase, normalized to the aqueous phase volume approximately 142 AU) was achieved by cell suspension culture in peanut oil-water two-phase system. Furthermore, the utilization of edible oil as extractant also fulfills the demand for application of Monascus pigments as natural food colorant.

  10. Preparation and properties of lauric acid/silicon dioxide composites as form-stable phase change materials for thermal energy storage

    Energy Technology Data Exchange (ETDEWEB)

    Fang Guiyin, E-mail: gyfang@nju.edu.cn [Department of Physics, Nanjing University, Hankou Road 22, Nanjing, Jiangsu 210093 (China); Li Hui [Department of Material Science and Engineering, Nanjing University, Nanjing 210093 (China); Liu Xu [Department of Physics, Nanjing University, Hankou Road 22, Nanjing, Jiangsu 210093 (China)

    2010-08-01

    Form-stable lauric acid (LA)/silicon dioxide (SiO{sub 2}) composite phase change materials were prepared using sol-gel methods. The LA was used as the phase change material for thermal energy storage, with the SiO{sub 2} acting as the supporting material. The structural analysis of these form-stable LA/SiO{sub 2} composite phase change materials was carried out using Fourier transformation infrared spectroscope (FT-IR). The microstructure of the form-stable composite phase change materials was observed by a scanning electronic microscope (SEM). The thermal properties and thermal stability were investigated by a differential scanning calorimeter (DSC) and a thermogravimetric analysis apparatus (TGA), respectively. The SEM results showed that the LA was well dispersed in the porous network of SiO{sub 2}. The DSC results indicated that the melting latent heat of the form-stable composite phase change material is 117.21 kJ kg{sup -1} when the mass percentage of the LA in the SiO{sub 2} is 64.8%. The results of the TGA showed that these materials have good thermal stability. The form-stable composite phase change materials can be used for thermal energy storage in waste heat recovery and solar heating systems.

  11. A microdevice assisted approach for the preparation, characterization and selection of continuous aqueous two-phase systems: from micro to bench-scale.

    Science.gov (United States)

    Vázquez-Villegas, Patricia; Ouellet, Eric; González, Claudia; Ruiz-Ruiz, Federico; Rito-Palomares, Marco; Haynes, Charles A; Aguilar, Oscar

    2016-07-05

    Aqueous two-phase systems (ATPS) have emerged as an alternative strategy for the recovery and purification of a wide variety of biological products. Typical process development requires a large screening of experimental conditions towards industrial adoption where continuous processes are preferred. In this work, it was proved that under certain flow conditions, ATPS could be formed continuously inside a microchannel, starting from stocks of phase components. Staggered herringbone chaotic micromixers included within the device sequentially and rapidly prepare two-phase systems across an entire range of useful phase compositions. Two-phase diagrams (binodal curves) were easily plotted using the cloud-point method for systems of different components and compared with previously reported curves for each system, proving that phase formation inside the device correlated with the previously reported diagrams. A proof of concept for sample partitioning in such a microdevice was performed with two different experimental models: BSA and red blood cells. Finally, the microdevice was employed to obtain information about the recovery and partition coefficient of invertase from a real complex mixture of proteins (yeast extract) to design a process for the recovery of the enzyme selecting a suitable system and composition to perform the process at bench-scale.

  12. Tuning crystal phase of NiSx through electro-oxidized nickel foam: A novel route for preparing efficient electrocatalysts for oxygen evolution reaction

    Science.gov (United States)

    Li, Xiao; Shang, Xiao; Rao, Yi; Dong, Bin; Han, Guan-Qun; Hu, Wen-Hui; Liu, Yan-Ru; Yan, Kai-Li; Chi, Jing-Qi; Chai, Yong-Ming; Liu, Chen-Guang

    2017-02-01

    A facile solvothermal sulfurization using electro-oxidized nickel foam (NF(Ox)) as support has been applied to prepare NiSx/NF(Ox) electrocatalyst with highly efficient activity for oxygen evolution reaction (OER). XRD patterns confirm the composition of NiSx/NF(Ox): two kinds of crystal phase including β-NiS and Ni3S2. While using bare NF as support under identical conditions, only Ni3S2 phase can be detected. SEM images reveal two kinds of morphologies of NiSx/NF(Ox) including pyramids structure of β-NiS and nanorod-like structure of Ni3S2, which implies the tuning effect of electro-pretreatment of NF on the selective preparation of NiSx crystal phase. It can be speculated that Ni(OH)2 layer derived from electro-oxidized NF is responsible for the growth of β-NiS while metallic Ni is transformed into Ni2S3 during sulfurization. Electrochemical measurements for OER indicate the enhanced electrocatalytic activity of NiSx/NF(Ox) with a small overpotential of 72 mV to reach 10 mA cm-2 compared with Ni3S2/NF, which may be ascribed to the improved electron-transfer kinetics relating to the unique atomic configurations and crystalline structures of β-NiS. The electro-oxidation pretreatment of nickel foam provides a simple and convenient method by tuning different NiSx crystal phases for preparing excellent OER eletrocatalysts.

  13. Visit at CERN of representatives of the Department of Piacenza (Italy), received by Lucio Rossi and Ugo Amaldi and hosted by the DG. The department of Piacenza is the native land of Edoardo Amaldi, one of the founding fathers of CERN, and the Department is preparing the celebration of the centennial of his birth.

    CERN Document Server

    Maximilien Brice

    2008-01-01

    Visit at CERN of representatives of the Department of Piacenza (Italy), received by Lucio Rossi and Ugo Amaldi and hosted by the DG. The department of Piacenza is the native land of Edoardo Amaldi, one of the founding fathers of CERN, and the Department is preparing the celebration of the centennial of his birth.

  14. Education and Job Training: Preparing for the 21st Century Workforce. Hearing before the Subcommittee on 21st Century Competitiveness of the Committee on Education and the Workforce, House of Representatives. One Hundred Seventh Congress, Second Session (Angola, Indiana, March 22, 2002).

    Science.gov (United States)

    Congress of the U.S., Washington, DC. House Committee on Education and the Workforce.

    This is a congressional hearing on how vocational and technical education and job training work together to better prepare workers for the 21st century workforce and on successful educational and job training activities and initiatives in Indiana (IN). Testimony includes statements from United States representatives (Howard P. "Buck"…

  15. Effects of chronic exposure to low-level pollutants in the environment. Prepared for the Subcommittee on the Environment and the Atmosphere of the Committee on Science and Technology, US House of Representatives, Ninety-Fourth Congress, First Session by the Congressional Research Service, Library of Congress, Serial 0

    Energy Technology Data Exchange (ETDEWEB)

    1975-01-01

    This report was prepared for the Subcommittee on the Environment and the Atmosphere of the US House of Representatives Committee on Science and Technology. It describes the effects of low-level, persistent pollutants on human health, fish and wildlife, agriculture, and climate.

  16. Preparation and chromatographic evaluation of a newly designed steviol glycoside modified-silica stationary phase in hydrophilic interaction liquid chromatography and reversed phase liquid chromatography.

    Science.gov (United States)

    Liang, Tu; Fu, Qing; Shen, Aijin; Wang, Hui; Jin, Yu; Xin, Huaxia; Ke, Yanxiong; Guo, Zhimou; Liang, Xinmiao

    2015-04-03

    A diterpene glycoside compound, rebaudioside A (commonly abbreviated as RA), was immobilized onto porous silica surface through "thiol-ene" click chemistry strategy. The successful immobilization of the RA on the silica support was confirmed by FT-IR and elemental analysis. Chromatographic characteristics of the new stationary phase, named Click TE-RA, were evaluated by a set of diverse analytes such as carbohydrates, nucleosides, and organic acids in hydrophilic interaction liquid chromatography (HILIC) mode. The effects of water content, buffer pH and concentration were investigated and a typical HILIC retention feature of Click TE-RA was observed at high organic modifier content. The Click TE-RA stationary phase was further studied by a series of glycoside compounds. Tunable retention mechanisms from hydrophilic to hydrophobic interactions were observed. Separation of very polar compounds including oligosaccharides, nucleic acid bases and nucleosides using Click TE-RA in HILIC mode was successfully accomplished. In addition, separation of saponins both in HILIC and reversed-phase liquid chromatography (RPLC) modes was performed, demonstrating the presence of orthogonality between two different modes on Click TE-RA column. The multiple interactions induced by polar sugar group and hydrophobic aglycone group allowed this Click TE-RA to serve as a multi-mode stationary phase in two-dimensional liquid chromatography.

  17. Chitosan-Coated Magnetic Nanoparticles Prepared in One-Step by Precipitation in a High-Aqueous Phase Content Reverse Microemulsion

    Directory of Open Access Journals (Sweden)

    María Guadalupe Pineda

    2014-07-01

    Full Text Available Chitosan-coated magnetic nanoparticles (CMNP were prepared in one-step by precipitation in a high-aqueous phase content reverse microemulsion in the presence of chitosan. The high-aqueous phase concentration led to productivities close to 0.49 g CMNP/100 g microemulsion; much higher than those characteristic of precipitation in reverse microemulsions for preparing magnetic nanoparticles. The obtained nanoparticles present a narrow particle size distribution with an average diameter of 4.5 nm; appearing to be formed of a single crystallite; furthermore they present superparamagnetism and high magnetization values; close to 49 emu/g. Characterization of CMNP suggests that chitosan is present as a non-homogeneous very thin layer; which explains the slight reduction in the magnetization value of CMNP in comparison with that of uncoated magnetic nanoparticles. The prepared nanoparticles show high heavy ion removal capability; as demonstrated by their use in the treatment of Pb2+ aqueous solutions; from which lead ions were completely removed within 10 min.

  18. Preparation of single phase Zn2TiO4 spinel from a new ZnTi layered double hydroxide precursor.

    Science.gov (United States)

    Song, Jianye; Leng, Mingzhe; Xiao, Hongdi; Zhang, Liangji; Qin, Yaowei; Hou, Wanguo; Du, Na; Liu, Jianqiang

    2014-06-01

    A single-source ZnTi-layered double hydroxide precursor was used to prepare single phase Zn2TiO4. This approach involves two steps: the calcination of a ZnTi-layered double hydroxide precursor and selective leaching zinc oxide from the resultant calcined products. The materials were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) thermogravimetric and differential thermal analysis (TG-DTA), transmission electron microscope (TEM), surface area measurement and UVvis diffuse reflection spectroscopy. The results indicated that a single phase Zn2TiO4 could be successfully obtained from a ZnTi-layered double hydroxide precursor at a relatively low temperature in short calcination time. The TEM and SEM show that the diameter of Zn2TiO4 particles prepared at 900 degrees C is in the range of 20-100 nm and smaller than that prepared by the solid-state method. UV-Vis diffuse reflection spectroscopy demonstrates that the material has an energy bandgap around 3.7 eV.

  19. Compression Effects on the Phase Behaviour of Miconazole-Poly (1-Vinylpyrrolidone-Co-Vinyl Acetate) Solid Dispersions-Role of Pressure, Dwell Time, and Preparation Method.

    Science.gov (United States)

    Singh, Abhishek; De Bisschop, Cathérine; Schut, Henk; Van Humbeeck, Jan; Van Den Mooter, Guy

    2015-10-01

    Compression of miconazole-poly (1-vinylpyrrolidone-co-vinyl acetate) (PVPVA64) solid dispersions prepared by spray drying and hot-melt extrusion was performed to gain insights into effect of compression pressure, dwell time, and preparation method on compression-dependent phase behavior. The solid dispersions prepared by spray drying were initially phase-separated showing two glass transition temperature (Tg), whereas the extruded samples showed one single Tg indicating better mixing. Compression caused mixing of spray-dried solid dispersions at high compression pressures and especially high dwell times. The extruded systems showed no statistically significant differences. However, physical mixtures made up from extruded samples containing 20% and 40% of active pharmaceutical ingredient underwent mixing upon compression. Coincidence Doppler measurements were performed to quantify the free volume of PVPVA64 which is a major contributor to the free volume in the solid dispersion matrix. A small but significant difference was found between the open free volume of the pure polymer subjected to varied manufacturing processes. Compression-induced plastic deformation and plastic flow enhances molecular mobility leading to mixing of different domains in solid dispersions. Different manufacturing methods may result in products with similar free volume, thereby showing similar molecular mobility.

  20. Preparation of cold ions in strong magnetic field and its application to gas-phase NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Fuke, K., E-mail: fuke@kobe-u.ac.jp [Institute for Molecular Science (Japan); Ohshima, Y. [Tokyo Institute of Technology, Department of Chemistry (Japan); Tona, M. [Ayabo Co. Fukukama (Japan)

    2015-11-15

    Nuclear Magnetic Resonance (NMR) technique is widely used as a powerful tool to study the physical and chemical properties of materials. However, this technique is limited to the materials in condensed phases. To extend this technique to the gas-phase molecular ions, we are developing a gas-phase NMR apparatus. In this note, we describe the basic principle of the NMR detection for molecular ions in the gas phase based on a Stern-Gerlach type experiment in a Penning trap and outline the apparatus under development. We also present the experimental procedures and the results on the formation and the manipulation of cold ions under a strong magnetic field, which are the key techniques to detect the NMR by the present method.

  1. Preparation of cold ions in strong magnetic field and its application to gas-phase NMR spectroscopy

    Science.gov (United States)

    Fuke, K.; Ohshima, Y.; Tona, M.

    2015-11-01

    Nuclear Magnetic Resonance (NMR) technique is widely used as a powerful tool to study the physical and chemical properties of materials. However, this technique is limited to the materials in condensed phases. To extend this technique to the gas-phase molecular ions, we are developing a gas-phase NMR apparatus. In this note, we describe the basic principle of the NMR detection for molecular ions in the gas phase based on a Stern-Gerlach type experiment in a Penning trap and outline the apparatus under development. We also present the experimental procedures and the results on the formation and the manipulation of cold ions under a strong magnetic field, which are the key techniques to detect the NMR by the present method.

  2. Study on Rare Earth-Containing Phases in TiAl Based Alloys Prepared by Non-Equilibrium Solidification Processing

    Institute of Scientific and Technical Information of China (English)

    马学著; 沈军; 贾均

    2001-01-01

    Microstructure evolution of rare earth rich phase of rapidly-solidified (RS) TiAl based alloys was investigated. The two rapid-solidification techniques employed are melt-spinning technique (MS) and Hammer-and-Anvil technique (HA). MS ribbons and HA foils were obtained in the experiment. The results demonstrate that with the increasing of cooling rates of TiAl based alloys great changes are taken place in the microstructures of rare earth rich phase, from scattering mainly on grain boundaries of as-cast ingot to distributing homogeneously as very fine fibers or powders (nanometer grade) on the matrix. The fine paralleling second phase fibers in the HA foils are considered to be connected with γ/α2 lamellar colonies. Selected area electronic diffraction (SAED) patterns of the rare earth rich phase is in accordance with that of intermetallic AlCe.

  3. Vertical phase separation of 6,13-bis(triisopropylsilylethynyl) pentacene/poly(methyl methacrylate) blends prepared by electrostatic spray deposition for organic field-effect transistors

    Science.gov (United States)

    Onojima, Norio; Hara, Kazuhiro; Nakamura, Ayato

    2017-05-01

    Blend films composed of 6,13-bis(triisopropylsilylethynyl) pentacene (TIPS pentacene) and poly(methyl methacrylate) (PMMA) were prepared by electrostatic spray deposition (ESD). ESD is considered as an intermediate process between dry and wet processes since the solvent present in small droplets can almost be evaporated before arriving at the substrate. Post-drying treatments with the time-consuming evaporation of residual solvents can be omitted. However, it is still not clear that a vertically phase-separated structure can be formed in the ESD process since the vertical phase separation of the blend films is associated with the solvent evaporation. In this study, we fabricated bottom-gate, top-contact organic field-effect transistors based on the blend films prepared by ESD and the devices exhibited transistor behavior with small hysteresis. This result demonstrates that the vertical phase separation of a blend film (upper TIPS pentacene active layer/bottom PMMA gate insulator) can occur in the facile one-step ESD process.

  4. Effect of doped SiO2 and calcinations temperature on phase transformation of TiO2 photocatalyst prepared by sol-gel method

    Directory of Open Access Journals (Sweden)

    Sutham Niyomwas

    2008-05-01

    Full Text Available The purpose of this research was to study the effect of calcinations temperature and SiO2 addition on phase transformation,crystallite size, and photocatalytic activity of SiO2/TiO2 thin films by using indigo carmine as an indicator. Thecomposite particles were prepared by sol-gel method via calcinations at a temperature range of 300-700oC for 2 h, and thecomposite thin films were prepared by means of spin coating. The microstructure and crystallite size of pure TiO2 and SiO2/TiO2 composite powders were characterized by using XRD, SEM and DTA. It was found that anatase structures wereformed at a calcinations temperature range of 300-600oC and mixed phases of anatase and rutile were observed at a temperatureof 700oC. Crystallite size of pure TiO2 tends to increase with an increase in calcinations temperature. Doped SiO2in the TiO2 has an effect on crystal phases and crystallite size of the composite powders and thin films, resulting in thechange of the photocatalytic activity of TiO2.

  5. Nanocrystalline TiO2 preparation by microwave route and nature of anatase–rutile phase transition in nano TiO2

    Indian Academy of Sciences (India)

    G M Neelgund; S A Shivashankar; B K Chethana; P P Sahoo; K J Rao

    2011-10-01

    Nanopowders of TiO2 has been prepared using a microwave irradiation-assisted route, starting from a metalorganic precursor, bis(ethyl-3-oxo-butanoato)oxotitanium (IV), [TiO(etob)2]2. Polyvinylpyrrolidone (PVP) was used as a capping agent. The as-prepared amorphous powders crystallize into anatase phase, when calcined. At higher calcination temperature, the rutile phase is observed to form in increasing quantities as the calcination temperature is raised. The structural and physicochemical properties were measured using XRD, FT–IR, SEM, TEM and thermal analyses. The mechanisms of formation of nano-TiO2 from the metal–organic precursor and the irreversible phase transformation of nano TiO2 from anatase to rutile structure at higher temperatures have been discussed. It is suggested that a unique step of initiation of transformation takes place in Ti1/2O layers in anatase which propagates. This mechanism rationalizes several key observations associated with the anatase–rutile transformation.

  6. Rapid microwave-assisted sol-gel preparation of Pd-substituted LnFeO3 (Ln = Y, La): phase formation and catalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Misch, Lauren M.; Birkel, Alexander; Figg, C. Adrian; Fors, Brett P.; Hawker, Craig J.; Stucky, Galen D.; Seshadri, Ram [UCSB

    2014-02-13

    We present a rapid microwave-assisted sol–gel approach to Pd-substituted LnFeO3 (Ln = Y, La) for applications in C–C coupling reactions. These materials could be prepared in household microwave ovens in less than 15 minutes of reaction time with the final materials displaying well-defined structure and morphology. Phase evolution was studied using time-dependent microwave heatings and then compared with the results obtained from thermogravimetric analyses. Materials were confirmed to be phase pure by laboratory and synchrotron X-ray diffraction. Substituted Pd is ionic as shown by the binding energy shift from X-ray photoelectron spectroscopy. The short heating periods required for phase purity allow these materials less time for sintering as compared to conventional solid state preparation methods, making relatively high surface areas achievable. These materials have been successfully used as catalyst precursor materials for C–C coupling reactions in which the active species is Pd0. Pd-substituted LnFeO3 (Ln = Y, La) provides Pd0 in solution which can be complexed by the ligand SPhos, allowing for aryl chloride coupling.

  7. Characteristics of PVdF-HFP/TiO{sub 2} composite membrane electrolytes prepared by phase inversion and conventional casting methods

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Kwang Man; Ryu, Kwang Sun; Chang, Soon Ho [Ionics Devices Team, Basic Research Lab., Electronics and Telecommunications Research Institute (ETRI), 161 Gajong, Yusong, Daejon 305-700 (Korea, Republic of); Park, Nam-Gyu [Materials Science and Technology Division, Korea Institute of Science and Technology (KIST), 39-1 Hwaolgok, Seongbuk, Seoul 136-791 (Korea, Republic of)

    2006-08-15

    Porous poly(vinylidene fluoride-co-hexafluoropropylene) (PVdF-HFP)-based polymer membranes filled with various contents of titania (TiO{sub 2}) nanocrystalline particles are prepared by phase inversion technique and, along with conventional casting method for comparison. N-methyl-2-pyrrolidone (NMP) as a solvent is used to dissolve the polymer and to make the slurry with TiO{sub 2}. Cast film is obtained by spreading the slurry and evaporating NMP in a dry oven, while phase inversion membrane by promptly immersing the spread slurry into flowing water as a non-solvent. Physical and electrochemical characterizations, such as morphology, thermal and crystalline behavior, and other transport properties of lithium ionic species, are carried out for the polymer films/membranes and the polymer electrolytes with absorbing an electrolyte solution. Phase inversion polymer electrolytes are proved to show superior behaviors in electrochemical properties, such as ionic conductivity, electrochemical and interfacial stability, than cast film electrolytes. This is greatly owed to highly porous structure of phase inversion membranes. Even including the feature of interfacial resistance with lithium electrode, phase inversion polymer electrolytes of PVdF-HFP/(5-20wt.% TiO{sub 2}) can be optimized as the adequate ones in applying to the electrolyte medium of lithium rechargeable batteries. (author)

  8. Thermal stability of alumina thin films containing {gamma}-Al{sub 2}O{sub 3} phase prepared by reactive magnetron sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Musil, J., E-mail: musil@kfy.zcu.cz [Department of Physics, Faculty of Applied Sciences, University of West Bohemia, Univerzitni 22, CZ-306 14 Plzen (Czech Republic); Institute of Physics, Academy of Sciences of the Czech Republic, Na Slovance 2, CZ-182 21 Praha 8 (Czech Republic); Blazek, J.; Zeman, P.; Proksova, S.; Sasek, M.; Cerstvy, R. [Department of Physics, Faculty of Applied Sciences, University of West Bohemia, Univerzitni 22, CZ-306 14 Plzen (Czech Republic)

    2010-11-15

    The paper reports on thermal stability of alumina thin films containing {gamma}-Al{sub 2}O{sub 3} phase and its conversion to a thermodynamically stable {alpha}-Al{sub 2}O{sub 3} phase during a post-deposition equilibrium thermal annealing. The films were prepared by reactive magnetron sputtering and subsequently post-deposition annealing was carried out in air at temperatures ranging from 700 deg. C to 1150 deg. C and annealing times up to 5 h using a thermogravimetric system. The evolution of the structure was investigated by means of X-ray diffraction after cooling down of the films. It was found that (1) the nanocrystalline {gamma}-Al{sub 2}O{sub 3} phase in the films is thermally stable up to 1000 deg. C even after 5 h of annealing, (2) the nanocrystalline {theta}-Al{sub 2}O{sub 3} phase was observed in a narrow time and temperature region at {>=}1050 deg. C, and (3) annealing at 1100 deg. C for 2 h resulted in a dominance of the {alpha}-Al{sub 2}O{sub 3} phase only in the films with a sufficient thickness.

  9. Preparation of a novel weak cation exchange/hydrophobic interaction chromatography dual-function polymer-based stationary phase for protein separation using "thiol-ene click chemistry".

    Science.gov (United States)

    Yang, Fan; Bai, Quan; Zhao, Kailou; Gao, Dong; Tian, Lei

    2015-02-01

    A novel dual-function mixed-mode stationary phase based on poly(glycidyl methacrylate-co-ethylene dimethacrylate) microspheres was synthesized by thiol-ene click chemistry and characterized by infrared spectroscopy and elemental analysis. The new system displays both hydrophobic interaction chromatography (HIC) character in a high salt concentration mobile phase, and weak cation exchange (WCX) chromatography character in a low salt concentration mobile phase. It can be used to separate proteins in both ion-exchange chromatography (IEC) mode and HIC mode. The resolution and selectivity of the stationary phase were evaluated in both HIC mode and IEC mode using protein standards. In comparison with the conventional WCX and HIC columns, the results were satisfactory and acceptable. Protein mass and bioactivity recoveries of more than 96% can be achieved in both HIC mode and IEC mode using this column. The results indicate that the novel dual-function mixed-mode column in many cases can replace the use of two individual WCX and HIC columns. In addition, the effects on protein separation of different ligand structures in the dual-function stationary phase and the pH of the mobile phase used were also investigated in detail. The results show that electrostatic interaction of the ligand with proteins must match the hydrophobicity of the ligand, which is an important factor to prepare the dual-function stationary phase. On the basis of this dual-function mixed-mode chromatography column, a new two-dimensional liquid chromatography technology with a single column system was also developed in this study, and was used to renature and purify recombinant human interferon-γ from inclusion bodies. The mass recovery, purity, and specific bioactivity obtained for the purified recombinant human interferon-γ were 87.2%, 92.4%, and 2.8 × 10(7) IU/mg, respectively, in IEC mode, and 83.4%, 95.2%, and 4.3 × 10(7) IU/mg, respectively, in HIC mode. The results indicate that the

  10. Aqueous phase preparation of ultrasmall MoSe2 nanodots for efficient photothermal therapy of cancer cells

    Science.gov (United States)

    Yuwen, Lihui; Zhou, Jiajia; Zhang, Yuqian; Zhang, Qi; Shan, Jingyang; Luo, Zhimin; Weng, Lixing; Teng, Zhaogang; Wang, Lianhui

    2016-01-01

    Photothermal therapy (PTT) is a promising cancer treatment with both high effectiveness and fewer side effects. However, an ideal PTT agent not only needs strong absorption of near-infrared (NIR) light and high photothermal conversion efficiency, but also needs good biocompatibility, stability, and small size, which makes the design and preparation of a novel PTT agent a great challenge. In this work, we developed an ultrasonication-assisted liquid exfoliation method for the direct preparation of ultrasmall (2-3 nm) MoSe2 nanodots (NDs) in aqueous solution and demonstrated their superior properties as a PTT agent. The as-prepared MoSe2 NDs have strong absorption of NIR light and high photothermal conversion efficiency of about 46.5%. In vitro cellular experiments demonstrate that MoSe2 NDs have negligible cytotoxicity and can efficiently kill HeLa cells (human cervical cell line) under NIR laser (785 nm) irradiation.Photothermal therapy (PTT) is a promising cancer treatment with both high effectiveness and fewer side effects. However, an ideal PTT agent not only needs strong absorption of near-infrared (NIR) light and high photothermal conversion efficiency, but also needs good biocompatibility, stability, and small size, which makes the design and preparation of a novel PTT agent a great challenge. In this work, we developed an ultrasonication-assisted liquid exfoliation method for the direct preparation of ultrasmall (2-3 nm) MoSe2 nanodots (NDs) in aqueous solution and demonstrated their superior properties as a PTT agent. The as-prepared MoSe2 NDs have strong absorption of NIR light and high photothermal conversion efficiency of about 46.5%. In vitro cellular experiments demonstrate that MoSe2 NDs have negligible cytotoxicity and can efficiently kill HeLa cells (human cervical cell line) under NIR laser (785 nm) irradiation. Electronic supplementary information (ESI) available: Characterization, size distribution and EDS spectrum of MoSe2 NDs, calculation of

  11. Preparation, characterization, and analytical applications of a novel polymer stationary phase with embedded or grafted carbon fibers.

    Science.gov (United States)

    Zhong, Yingying; Zhou, Wenfang; Zhang, Peimin; Zhu, Yan

    2010-09-15

    A polymer-based chromatographic stationary phase with embedded or grafted multi-walled carbon nanotubes (MWCNTs) has been developed. Three different synthetic methods were utilized to combine the nano-fibers with the substrate of polystyrene-divinylbenzene (PS-DVB). After optimizing the synthetic conditions, this novel polystyrene-divinylbenzene-carbon nanotube (PS-DVB-CNT) stationary phase was characterized by scanning electron microscopy, Raman spectroscopy, thermogravimetric analysis, chemical adsorption and desorption measurement, and mechanical stability test. Compared to PS-DVB particles, PS-DVB-CNT particles have certain improvement in physical and chromatographic performances because the addition of MWCNTs has altered the structures of the particles. The novel stationary phase owns satisfactory resolution, wide pH endurance, and long lifetime, which can be used as an extent to normal HPLC.

  12. Preparation of Si sub 1 sub - sub x sub - sub y Ge sub x C sub y semiconductor films on Si by ion implantation and solid phase epitaxy

    CERN Document Server

    Liu Xue Qin; Zhen Cong Mian; Zhang Jing; Yang Yi; Guo Yong

    2002-01-01

    Si sub 1 sub - sub x sub - sub y Ge sub x C sub y ternary alloy semiconductor films were prepared on Si(100) substrates by C ion implanting SiGe films and subsequent solid phase epitaxy (SPE). Two-step annealing technique was employed in the SPE processing. The properties of the alloy films were determined using Rutherford backscattering spectroscopy (RBS), Fourier transform infrared spectroscopy (FTIR) and High-resolution x-ray diffraction (HRXRD) measurements. It is shown that C atoms are located at substitutional sites and the incorporation of C relieves the compressive strain in the SiGe layer

  13. Synthesis and Electrochemical Studies on Spinel Phase LiMn2O4 Cathode Materials Prepared by Different Processes

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    Three kinds of processes, high temperature solid state reaction, precipitation and sol-gel technique were used to synthsize spinel phase LiMn2O4. XRD, DTA-TG results show that phase-pure spinel LiMn2O4 could be synthesized under the lowest calcined temperature by the sol-gel technique compared to the precipitation method and solid state reaction. BET, SEM and electrochemical measurements results demonstrate that the features of the powders affect directly the electrochemical capacities; large specific area and small homogeneous grain size are of advantage for the lithium ion insertion and extraction in the charge and discharge process.

  14. Characterization of Polyamide 66 membranes prepared by phase inversion using formic acid and hydrochloric acid such as solvents

    Directory of Open Access Journals (Sweden)

    Patrícia Poletto

    2011-12-01

    Full Text Available The membranes properties prepared from water/formic acid (FA/ polyamide 66 (PA66 and water/hydrochloric acid (HCl/polyamide 66 (PA 66 systems has been studied. The different solvents interact distinctly with the polymer, affecting the membrane morphology. The asymmetric structure of the membranes showed a dense top layer and a porous sublayer. The membranes M-HCl prepared from HCl/PA 66 system showed a larger dense layer (around 23 μm in compared to those prepared from FA/PA 66 system (M-FA (around 10 μm. The membrane morphology was a determinant factor in results of water absorption, porosity and pure water flux. The lower thickness of dense layer in M-FA membranes resulted in a higher water absorption and, consequently, porosity, approximately 50%, compared with M-HCl membranes, approximately 15%. The same trend was observed to permeate flux, the lower thickness of dense layer higher pure water flux.

  15. Effects of Additive AlCl3 on Crystal Phase, Particle Size and Microstructural Parameters of Nanocrystalline TiO2 Prepared by HF-PCVD

    Institute of Scientific and Technical Information of China (English)

    Haiping XU; Yanping SUN; Xinmou CHEN

    2004-01-01

    Nanocrystalline TiO2 was prepared by high frequency plasma chemical vapor deposition (HF-PCVD). The effects of additive AlCl3 on crystal phase, particle size and microstructural parameters of TiO2 nanocrystallites were investigated by X-ray diffraction(XRD) and transmission electron microscopy (TEM). The nanocrystallites obtained experimentally are mixture of anatase and rutile, the uniform diameters of particles are about 30 nm. The phase transformation from anatase to rutile was accelerated by AlCl3, and rutile content is increased from 26.7 wt pct to 53.6 wt pct with increasing of addition of AlCl3 from 0.0 wt pct to 5.0 wt pct. The particle size is reduced and the size distribution becomes very narrow. The crystal lattice constants have the trend to decrease, and cell volumes appear as shrinkable.

  16. Creating Drug Solubilization Compartments via Phase Separation in Multicomponent Buccal Patches Prepared by Direct Hot Melt Extrusion-Injection Molding

    NARCIS (Netherlands)

    Alhijjaj, Muqdad; Bouman, Jacob; Wellner, Nikolaus; Belton, Peter; Qi, Sheng

    2015-01-01

    Creating in situ phase separation in solid dispersion based formulations to allow enhanced functionality of the dosage form, such as improving dissolution of poorly soluble model drug as well as being mucoadhesive, can significantly maximize the in vitro and in vivo performance of the dosage form

  17. Phase equilibrium and preparation, crystallization and viscous sintering of glass in the alumina-silica-lanthanum phosphate system

    Science.gov (United States)

    He, Feng

    The phase equilibrium, viscosity of melt-quenched glasses, and processing of sol-gel glasses of the alumina-silica-lanthanum phosphate system were studied. These investigations were directed towards serving the objective of synthesizing nano-structured ceramic-matrix-composites via controlled crystallization of glass precursors. The thermal stability, phase equilibrium, and liquidus temperatures of the alumina- and mullite-lanthanum phosphate systems are determined. An iridium wire heater was constructed to anneal samples up to 2200°C. Phosphorus evaporation losses were significant at high temperatures, especially over 1800°C. The tentative phase diagrams of the two quasi-binary systems were presented. The viscosity of the melt-quenched mullite-lanthanum phosphate glasses was measured by three different methods, including viscous sintering of glass powder compacts, neck formation between two Frenkel glass beads, and thermal analysis of the glass transition. Improved methodologies were developed for applying the interpretative mathematical models to the results of the sintered powder and thermal analytical experiments. Good agreement was found between all three methods for both absolute values and temperature dependence. A sol-gel process was developed as a low temperature route to producing glasses. A unique, single phase mullite gel capable of low temperature (575°C) mullitization was made from tetraethoxysilane and aluminum isopropoxide at room temperature in three days. Low temperature crystallization was attributed to the avoidance of phase segregation during gel formation and annealing. This was greatly enhanced by a combination of low temperature preheating in the amorphous state, a high heating rate during crystallization and low water content. The Al2O3 content in mullite (61-68 mol%) depended on the highest annealing temperature. Two mullite-lanthanum phosphate gels were made based upon modifying the chemical procedures used for the homogeneous single

  18. Dense and high-stability Ti2AlN MAX phase coatings prepared by the combined cathodic arc/sputter technique

    Science.gov (United States)

    Wang, Zhenyu; Liu, Jingzhou; Wang, Li; Li, Xiaowei; Ke, Peiling; Wang, Aiying

    2017-02-01

    Ti2AlN belongs to a family of ternary nano-laminate alloys known as the MAX phases, which exhibit a unique combination of metallic and ceramic properties. In the present work, the dense and high-stability Ti2AlN coating has been successfully prepared through the combined cathodic arc/sputter deposition, followed by heat post-treatment. It was found that the as-deposited Ti-Al-N coating behaved a multilayer structure, where (Ti, N)-rich layer and Al-rich layer grew alternately, with a mixed phase constitution of TiN and TiAlx. After annealing at 800 °C under vacuum condition for 1.5 h, although the multilayer structure still was found, part of multilayer interfaces became indistinct and disappeared. In particular, the thickness of the Al-rich layer decreased in contrast to that of as-deposited coating due to the inner diffusion of the Al element. Moreover, the Ti2AlN MAX phase emerged as the major phase in the annealed coatings and its formation mechanism was also discussed in this study. The vacuum thermal analysis indicated that the formed Ti2AlN MAX phase exhibited a high-stability, which was mainly benefited from the large thickness and the dense structure. This advanced technique based on the combined cathodic arc/sputter method could be extended to deposit other MAX phase coatings with tailored high performance like good thermal stability, high corrosion and oxidation resistance etc. for the next protective coating materials.

  19. Preparation and selective recognition of a novel solid-phase microextraction fiber combined with molecularly imprinted polymers for the extraction of parabens in soy sample.

    Science.gov (United States)

    He, Juan; Chen, Si; Jiang, Yili; Shen, Yanzheng; Zhu, Jing; Wei, Hongliang; Zhang, Hongxia; Lu, Kui

    2012-01-01

    A prepared molecularly imprinted polymer with ethyl p-hydroxybenzoate as template molecule was applied for the first time to a homemade solid-phase microextraction fiber. The molecularly imprinted polymer-coated solid-phase microextraction fiber was characterized by scanning electron microscopy and thermogravimetric analysis. Various parameters were investigated, including extraction temperature, extraction time, and desorption time. Under the optimum extraction conditions, the molecularly imprinted polymer-coated solid-phase microextraction fiber exhibited higher selectivity with greater extraction capacity toward parabens compared with the nonimprinted polymer-coated solid-phase microextraction fiber and commercial fibers. The molecularly imprinted polymer-coated solid-phase microextraction fiber was tested using gas chromatography to determine parabens, including methyl p-hydroxybenzoate, ethyl p-hydroxybenzoate, and propyl p-hydroxybenzoate. The linear ranges were 0.01-10 μg/mL with a correlation coefficient above 0.9943. The detection limits (under signal-to-noise ratio of 3) were below 0.30 μg/L. The fiber was successfully applied to the simultaneous analysis of three parabens in spiked soy samples with satisfactory recoveries of 95.48, 97.86, and 92.17%, respectively. The relative standard deviations (n=6) were within 2.83-3.91%. The proposed molecularly imprinted polymer-coated solid-phase microextraction method is suitable for selective extraction and determination of trace parabens in food samples. Copyright © 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Preparation and Performance Analysis of Na2SO4·10H2O/EG Composite Phase-change Materials

    Directory of Open Access Journals (Sweden)

    LENG Cong-bin

    2017-01-01

    Full Text Available Sodium sulfate decahydrate/expanded graphite composite phase-change material (Na2SO4·10H2O/EG was prepared by vacuum adsorption method.The thermal properties of Na2SO4·10H2O/EG,such as melting-solidification,phase separation,supercooling and latent heat were tested and analyzed.The results show that with the addition of 2%(mass fraction borax and 8% EG,the composite phase-change materials Na2SO4·10H2O/EG obtain ideal properties.The phase separation is eliminated,the supercooling degree of Na2SO4·10H2O is reduced from 13.6℃ to below 0.6℃,the latent heat and the energy storage density of the phase-change materials reach 225.77kJ·kg-1 and 218.09MJ·m-3 respectively.The thermal conductivity is also greatly improved.Compared with Na2SO4·10H2O with the addition of the nucleating agent borax only,the time for heat storage is shortened by 52.6%,and the time for heat release is shortened by 55.1%.Even after 500 times of rapid heating and cooling cycles,the performance of Na2SO4·10H2O/EG does not deteriorate.The novel composite phase-change material has better storage/exothermic properties.

  1. List of Accredited Representatives

    Data.gov (United States)

    Department of Veterans Affairs — VA accreditation is for the sole purpose of providing representation services to claimants before VA and does not imply that a representative is qualified to provide...

  2. The representative animal

    OpenAIRE

    Harrison, J M

    1994-01-01

    The anthropocentric approach to the study of animal behavior uses representative nonhuman animals to understand human behavior. This approach raises problems concerning the comparison of the behavior of two different species. The datum of behavior analysis is the behavior of humans and representative animal phenotypes. The behavioral phenotype is the product of the ontogeny and phylogeny of each species, and this requires that contributions of genotype as well as behavioral history to experim...

  3. [Advance directives. Representatives' opinions].

    Science.gov (United States)

    Busquets I Font, J M; Hernando Robles, P; Font I Canals, R; Diestre Ortin, G; Quintana, S

    The use and usefulness of Advance Directives has led to a lot of controversy about their validity and effectiveness. Those areas are unexplored in our country from the perspective of representatives. To determine the opinion of the representatives appointed in a registered Statement of Advance Directives (SAD) on the use of this document. Telephone survey of representatives of 146 already dead people and who, since February 2012, had registered a SAD document. More the two-thirds (98) of respondents recalled that the SAD was consulted, with 86 (58.9%) saying that their opinion as representative was consulted, and 120 (82.1%) believe that the patient's will was respected. Of those interviewed, 102 (69.9%) believe that patients who had previously planned their care using a SAD had a good death, with 33 (22.4%) saying it could have been better, and 10 (6.9%) believe they suffered greatly. The SAD were mostly respected and consulted, and possibly this is related to the fact that most of the representatives declare that the death of those they represented was perceived as comfortable. It would be desirable to conduct further studies addressed at health personnel in order to know their perceptions regarding the use of Advance Directives in the process of dying. Copyright © 2016 SECA. Publicado por Elsevier España, S.L.U. All rights reserved.

  4. Study of interaction of ethylene glycol/PVP phase on noble metal powders prepared by polyol process

    Indian Academy of Sciences (India)

    F Bonet; K Tekaia-Elhsissen; K Vijaya Sarathy

    2000-06-01

    Noble metal powders (Au, Ag, Pt, Pd and Ru) have been synthesized by the polyol process in both the nanometer and submicron scales (sans Pd, Pt and Ru). They have been characterized by both microscopic (TEM and SEM) as well as spectroscopic techniques (FT-IR and XPS). Infrared spectroscopy was employed to study the colloid particles in the presence of ethylene glycol and PVP and the results show that the interaction between the organic phase and the metal particles vary according to the particle size. The role of the solvent, ethylene glycol, during the reduction process was also investigated and we observe formation of >C=O vibration band after the reduction process implying that the solvent reduces the metal ions thereby getting oxidized. XPS measurements carried out on the colloidal sols have shown the presence of the organic phase adsorbed onto the metal particles.

  5. Nanoparticles of conjugated polymers prepared from phase-separated films of phospholipids and polymers for biomedical applications.

    Science.gov (United States)

    Yoon, Jungju; Kwag, Jungheon; Shin, Tae Joo; Park, Joonhyuck; Lee, Yong Man; Lee, Yebin; Park, Jonghyup; Heo, Jung; Joo, Chulmin; Park, Tae Jung; Yoo, Pil J; Kim, Sungjee; Park, Juhyun

    2014-07-09

    Phase separation in films of phospholipids and conjugated polymers results in nanoassemblies because of a difference in the physicochemical properties between the hydrophobic polymers and the polar lipid heads, together with the comparable polymer side-chain lengths to lipid tail lengths, thus producing nanoparticles of conjugated polymers upon disassembly in aqueous media by the penetration of water into polar regions of the lipid heads.

  6. Preparation and Mechanical Properties of Solid-phase Grafting Nanocomposites of PVC/Graft Copolymers/MMT

    Institute of Scientific and Technical Information of China (English)

    ZHOU Dunbai; CAI Changgen; JIA Demin

    2006-01-01

    In order to improve the mechanical properties of PVC, by solid-phase grafting reaction, grafting on and nano-modifying the PVC process synchronously, acrylic monomers not only graft on PVC, but also are intercalated into the layers of MMT in the heating process. Blending PVC and the MMT-PVC grafting copolymers, we can get nanocomposites of PVC/ grafters/ MMT, and the mechanical performance of the material is improved.

  7. Complexation induced phase separation: preparation of composite membranes with a nanometer thin dense skin loaded with metal ions

    KAUST Repository

    Villalobos Vazquez de la Parra, Luis Francisco

    2015-04-21

    We present the development of a facile phase-inversion method for forming asymmetric membranes with a precise high metal ion loading capacity in only the dense layer. The approach combines the use of macromolecule-metal intermolecular complexes to form the dense layer of asymmetric membranes with nonsolvent-induced phase separation to form the porous support. This allows the independent optimization of both the dense layer and porous support while maintaining the simplicity of a phase-inversion process. Moreover, it facilitates control over (i) the thickness of the dense layer throughout several orders of magnitude—from less than 15 nm to more than 6 μm, (ii) the type and amount of metal ions loaded in the dense layer, (iii) the morphology of the membrane surface, and (iv) the porosity and structure of the support. This simple and scalable process provides a new platform for building multifunctional membranes with a high loading of well-dispersed metal ions in the dense layer.

  8. Complexation-induced phase separation: preparation of composite membranes with a nanometer-thin dense skin loaded with metal ions.

    Science.gov (United States)

    Villalobos, Luis Francisco; Karunakaran, Madhavan; Peinemann, Klaus-Viktor

    2015-05-13

    We present the development of a facile phase-inversion method for forming asymmetric membranes with a precise high metal ion loading capacity in only the dense layer. The approach combines the use of macromolecule-metal intermolecular complexes to form the dense layer of asymmetric membranes with nonsolvent-induced phase separation to form the porous support. This allows the independent optimization of both the dense layer and porous support while maintaining the simplicity of a phase-inversion process. Moreover, it facilitates control over (i) the thickness of the dense layer throughout several orders of magnitude from less than 15 nm to more than 6 μm, (ii) the type and amount of metal ions loaded in the dense layer, (iii) the morphology of the membrane surface, and (iv) the porosity and structure of the support. This simple and scalable process provides a new platform for building multifunctional membranes with a high loading of well-dispersed metal ions in the dense layer.

  9. Preparation of LuAG Powders with Single Phase and Good Dispersion for Transparent Ceramics Using Co-Precipitation Method

    Directory of Open Access Journals (Sweden)

    Liangjie Pan

    2015-08-01

    Full Text Available The synthesis of pure and well dispersed lutetium aluminum garnet (LuAG powder is crucial and important for the preparation of LuAG transparent ceramics. In this paper, high purity and well dispersed LuAG powders have been synthesized via co-precipitation method with lutetium nitrate and aluminum nitrate as raw materials. Ammonium hydrogen carbonate (AHC was used as the precipitant. The influence of aging time, pH value, and dripping speed on the prepared LuAG powders were investigated. It showed that long aging duration (>15 h with high terminal pH value (>7.80 resulted in segregation of rhombus Lu precipitate and Al precipitate. By decreasing the initial pH value or accelerating the dripping speed, rhombus Lu precipitate was eliminated and pure LuAG nano powders were synthesized. High quality LuAG transparent ceramics with transmission >75% at 1064 nm were fabricated using these well dispersed nano LuAG powders.

  10. Preparation of solid-phase microextraction fiber coated with single-walled carbon nanotubes by electrophoretic deposition and its application in extracting phenols from aqueous samples.

    Science.gov (United States)

    Li, Quanlong; Wang, Xuefeng; Yuan, Dongxing

    2009-02-27

    A novel solid-phase microextraction (SPME) Pt fiber coated with single-walled carbon nanotubes (SWCNTs) was prepared by electrophoretic deposition (EPD) and applied to the determination of phenols in aqueous samples by direct immersion (DI)-SPME-HPLC-UV. The results revealed that EPD was a simple and reproducible technique for the preparation of SPME fibers coated with SWCNTs without the use of adhesive. The obtained SWCNT coating did not swell in organic solvents nor strip off from substrate, and possessed high mechanical strength due to the strong Van der Waals attractions between the surfaces of the SWCNTs. The prepared SPME fiber was conductive since both SWCNT coating and Pt wire were conductive. Using Pt wire as substrate, the fiber was unbreakable. Owing to the presence of oxygenated groups on SWCNTs and the high surface area of SWCNTs, the SWCNT fiber was similar to or superior to commercial PA fiber in extracting the studied phenols from aqueous sample. A durability of more than 80 analyses was achieved for one unique fiber. Under optimized conditions, the detection limits for the phenols varied between 0.9 and 3.8 ng/mL, the precisions were in the range of 0.7-3.2% (n=3), and linear ranges were within 10 and 300 ng/mL. The method was successfully applied to the analysis of spiked seawater and tap water samples with the recoveries from 87.5 to 102.0%.

  11. Online polar two phase countercurrent chromatography×high performance liquid chromatography for preparative isolation of polar polyphenols from tea extract in a single step.

    Science.gov (United States)

    Chen, Wei-Bin; Li, Shu-Qi; Chen, Long-Jiang; Fang, Mei-Juan; Chen, Quan-Cheng; Wu, Zhen; Wu, Yun-Long; Qiu, Ying-Kun

    2015-08-01

    Herein, we report an on-line two-dimensional system constructed by counter-current chromatography (CCC) coupling with preparative high-performance liquid chromatography (prep-HPLC) for the separation and purification of polar natural products. The CCC was used as the first dimensional isolation column, where an environmental friendly polar two-phase solvent system of isopropanol and 16% sodium chloride aqueous solution (1:1.2, v/v) was introduced for low toxicity and favorable resolution. In addition, by applying the stop-and-go flow technique, effluents pre-fractionated by CCC was further purified by a preparative column packed with octadecyl silane (ODS) as the second dimension. The interface between the two dimensions was comprised of a 6-port switching valve and an electronically controlled 2-position 10-port switching valve connected with two equivalent holding columns. To be highlighted here, this rationally designed interface for the purpose of smooth desalination, absorption and desorption, successfully solved the solvent compatibility problem between the two dimensional separation systems. The present integrated system was successfully applied in a one-step preparative separation and identification of 10 pure compounds from the water extracts of Tieguanyin tea (Chinese oolong tea). In short, all the results demonstrated that the on-line 2D CCC×LC method is an efficient and green approach for harvesting polar targets in a single step, which showed great promise in drug discovery. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. [[Chiral separation of five arylpropionic acid drugs and determination of their enantiomers in pharmaceutical preparations by reversed-phase high performance liquid chromatography with cellulose-tris-(4-methylbenzoate) stationary phase

    Science.gov (United States)

    Luo, An; Wan, Qiang; Fan, Huajun; Chen, Zhi; Wu, Xuehao; Huang, Xiaowen; Zang, Linquan

    2014-09-01

    Chromatographic behaviors for enantiomeric separation of arylpropionic acid drugs were systematically developed by reversed phase-high performance liquid chromatography (RP-HPLC) using cellulose-tris-(4-methylbenzoate) (CTMB) as chiral stationary phase (CSP). The effects of the composition of the mobile phase, additives and temperature on chiral separation of flurbiprofen, pranoprofen, naproxen, ibuprofen and loxoprofen were further investigated. The enantiomers had been successfully separated on CSP of CTMB by the mobile phase of methanol-0.1% (v/v) formic acid except naproxen by acetonitrile-0.1% (v/v) formic acid at 25 °C. The mechanisms of the racemic resolution for the above mentioned five drugs are discussed thermodynamically and structurally. The resolutions between respective enantiomers for arylpropionic acid drugs on CTMB had significant differences due to their chromatographic behaviors. The order of resolutions ranked pranoprofen, loxoprofen, flurbiprofen, ibuprofen and naproxen. The method established has been successfully applied to the determination of the enantiomers of the five drugs in commercial preparations under the optimized conditions. It proved that the method is simple, reliable and accurate.

  13. Representing properties locally.

    Science.gov (United States)

    Solomon, K O; Barsalou, L W

    2001-09-01

    Theories of knowledge such as feature lists, semantic networks, and localist neural nets typically use a single global symbol to represent a property that occurs in multiple concepts. Thus, a global symbol represents mane across HORSE, PONY, and LION. Alternatively, perceptual theories of knowledge, as well as distributed representational systems, assume that properties take different local forms in different concepts. Thus, different local forms of mane exist for HORSE, PONY, and LION, each capturing the specific form that mane takes in its respective concept. Three experiments used the property verification task to assess whether properties are represented globally or locally (e.g., Does a PONY have mane?). If a single global form represents a property, then verifying it in any concept should increase its accessibility and speed its verification later in any other concept. Verifying mane for PONY should benefit as much from having verified mane for LION earlier as from verifying mane for HORSE. If properties are represented locally, however, verifying a property should only benefit from verifying a similar form earlier. Verifying mane for PONY should only benefit from verifying mane for HORSE, not from verifying mane for LION. Findings from three experiments strongly supported local property representation and ruled out the interpretation that object similarity was responsible (e.g., the greater overall similarity between HORSE and PONY than between LION and PONY). The findings further suggest that property representation and verification are complicated phenomena, grounded in sensory-motor simulations.

  14. Preparation and thermal properties of form-stable palmitic acid/active aluminum oxide composites as phase change materials for latent heat storage

    Energy Technology Data Exchange (ETDEWEB)

    Fang, Guiyin, E-mail: gyfang@nju.edu.cn [School of Physics, Nanjing University, Nanjing 210093 (China); Li, Hui [Department of Material Science and Engineering, Nanjing University, Nanjing 210093 (China); Cao, Lei; Shan, Feng [School of Physics, Nanjing University, Nanjing 210093 (China)

    2012-12-14

    Form-stable palmitic acid (PA)/active aluminum oxide composites as phase change materials were prepared by adsorbing liquid palmitic acid into active aluminum oxide. In the composites, the palmitic acid was used as latent heat storage materials, and the active aluminum oxide was used as supporting material. Fourier transformation infrared spectroscope (FT-IR), X-ray diffractometer (XRD) and scanning electronic microscope (SEM) were used to determine the chemical structure, crystalloid phase and microstructure of the composites, respectively. The thermal properties and thermal stability were investigated by a differential scanning calorimeter (DSC) and a thermogravimetry analyzer (TGA). The FT-IR analyses results indicated that there is no chemical interaction between the palmitic acid and active aluminum oxide. The SEM results showed that the palmitic acid was well adsorbed into porous network of the active aluminum oxide. The DSC results indicated that the composites melt at 60.25 Degree-Sign C with a latent heat of 84.48 kJ kg{sup -1} and solidify at 56.86 Degree-Sign C with a latent heat of 78.79 kJ kg{sup -1} when the mass ratio of the PA to active aluminum oxide is 0.9:1. Compared with that of the PA, the melting and solidifying time of the composites CPCM5 was reduced by 20.6% and 21.4% because of the increased heat transfer rate through EG addition. The TGA results showed that the active aluminum oxide can improve the thermal stability of the composites. -- Highlights: Black-Right-Pointing-Pointer Form-stable PA/active aluminum oxide composites as PCMs were prepared. Black-Right-Pointing-Pointer Chemical structure, crystalloid phase and microstructure of composites were determined. Black-Right-Pointing-Pointer Thermal properties and thermal stability of the composites were investigated. Black-Right-Pointing-Pointer Expanded graphite can improve thermal conductivity of the composites.

  15. Representing and Performing Businesses

    DEFF Research Database (Denmark)

    Boll, Karen

    2014-01-01

    and MacKenzie’s idea of performativity. Based on these two approaches, the article demonstrates that the segmentation model represents and performs the businesses as it makes up certain new ways to be a business and as the businesses can be seen as moving targets. Inspired by MacKenzie the argument......This article investigates a segmentation model used by the Danish Tax and Customs Administration to classify businesses’ motivational postures. The article uses two different conceptualisations of performativity to analyse what the model’s segmentations do: Hacking’s notion of making up people...... is that the segmentation model embodies cleverness in that it simultaneously alters what it represents and then represents this altered reality to confirm the accuracy of its own model of the businesses’ postures. Despite the cleverness of the model, it also has a blind spot. The model assumes a world wherein everything...

  16. A series of spinel phase cathode materials prepared by a simple hydrothermal process for rechargeable lithium batteries

    Science.gov (United States)

    Liang, Yan-Yu; Bao, Shu-Juan; Li, Hu-Lin

    2006-07-01

    A series of spinel-structured materials have been prepared by a simple hydrothermal procedure in an aqueous medium. The new synthetic method is time and energy saving i.e., no further thermal treatment and extended grinding. The main experimental process involved the insertion of lithium into electrolytic manganese dioxide with glucose as a mild reductant in an autoclave. Both the hydrothermal temperature and the presence of glucose play the critical roles in determining the final spinel integrity. Particular electrochemical performance has also been systematically explored, and the results show that Al 3+, F - co-substituted spinels have the best combination of initial capacity and capacity retention among all these samples, exhibited the initial capacity of 115 mAh/g and maintained more than 90% of the initial value at the 50th cycle.

  17. Preparation and characterization of ceramic/carbon coated Fe₃O₄ magnetic nanoparticle nanocomposite as a solid-phase microextraction adsorbent.

    Science.gov (United States)

    Heidari, Hassan; Razmi, Habib; Jouyban, Abolghasem

    2012-07-06

    A novel solid-phase microextraction (SPME) fiber based on a glass tube coated with ceramic/carbon coated Fe₃O₄ magnetic nanoparticle nanocomposite (C-Fe₃O₄/C MNP) was prepared by sol-gel technique. The carbon coated Fe₃O₄ magnetic nanoparticles were synthesized by a simple hydrothermal reaction and the resultant powder was mixed with sol-gel precursors to prepare C-Fe₃O₄/C MNP. The prepared C-Fe₃O₄/C MNP was deposited on surface of glass tubes as new substrate with a simple method. The results revealed that this procedure was a simple and reproducible technique for the preparation of SPME fibers coated with magnetic nanoparticles. The scanning electron micrographs of the fiber surface revealed a three-dimensional structure which is suitable as SPME adsorbents. Some polycyclic aromatic hydrocarbons (PAHs) were selected as model compounds for evaluating performance of the designed SPME fiber. The analytes were extracted with SPME, and desorbed using acetonitrile via ultrasonication. The extracts were analyzed by high performance liquid chromatography (HPLC) with fluorescence detection. The results demonstrated that the proposed method based on the C-Fe₃O₄/C MNP fiber had wide dynamic linear range (0.01-350 μg L⁻¹) with good linearity (R²>0.990) and low detection limits (0.7-50 pg mL⁻¹). The relative standard deviation ranged from 6.9% to 12.2% for inter-day variations. These fibers were successfully used for the analysis of spiked water samples, which demonstrating the applicability of the home-made C-Fe₃O₄/C MNP fibers.

  18. Effect of oxidant on the performance of conductive polymer films prepared by vacuum vapor phase polymerization for smart window applications

    Science.gov (United States)

    Brooke, Robert; Fabretto, Manrico; Vucaj, Nastasja; Zuber, Kamil; Switalska, Eliza; Reeks, Lachlan; Murphy, Peter; Evans, Drew

    2015-03-01

    Conductive polymers synthesized by vacuum vapour phase polymerization (VPP) were investigated and optimized by changing the oxidant solution and VPP chamber parameters for their incorporation into ‘smart window’ electrochromic devices. Additionally, the interaction of two oxidant solutions with typical electrode materials (aluminium and indium tin oxide) were examined with respect to material etching, device cosmetics and long term device degradation (over 10 000 switch cycles). Devices made with conducting polymers synthesized with the oxidant Fe(Tos)3 rather than FeCl3 produced superior device performance with respect to optical switching range (%T), switch speed and optical relaxation.

  19. Preparation of starch stabilized silver nanoparticles with spatial self-phase modulation properties by laser ablation technique

    Energy Technology Data Exchange (ETDEWEB)

    Zamiri, Reza; Azmi, B.Z.; Sadrolhosseini, Amir R.; Husin, M.S.; Zaidan, A.W. [Universiti Putra Malaysia, Department of Physics, Faculty of Science, UPM Serdang, Selangor (Malaysia); Darroudi, Majid [Universiti Putra Malaysia, Advanced Materials and Nanotechnology Laboratory, Institute of Advanced Technology, UPM Serdang, Selangor (Malaysia); Mahdi, M.A. [Universiti Putra Malaysia, Wireless and Photonics Networks Research Center, Faculty of Engineering, UPM Serdang, Selangor (Malaysia)

    2011-01-15

    Silver nanoparticles inside the starch solution have been successfully fabricated by laser ablation of a silver plate immersed in starch solution. The ablation has been done using a Q-switched Nd:YAG laser at 10 Hz repetition rate. The starch solution allows for the formation of silver nanoparticles with uniform particle diameters and well dispersed. The ablation was performed at different time durations to study the influence of the laser ablation time on efficiency of particle formation and sizes. The Spatial Self-phase modulation phenomena which can determine the nonlinear optical property of the samples were also investigated for starch solutions containing silver nanoparticles. (orig.)

  20. Annotated bibliography on selected areas of coal mining research and development. Report prepared for the Committee on Science and Technology, US House of Representatives, Ninety-Sixth Congress, First Session by the Congressional Research Service, Library of Congress

    Energy Technology Data Exchange (ETDEWEB)

    1979-01-01

    The Congressional Research Service has completed an annotated bibliography on coal mining research and development. Although the completion of the study was delayed in order to permit CRS analysts to search the libraries of Bituminous Coal, Research Inc., and the Bureau of Mines in the Pittsburgh area, current re-emphasis on the use of coal as an energy source indicates a sustained relevance. The bibliography presents key references to coal-mining R and D under six subject headings keyed to issues of central concern in coal production: (1) mine health and safety, (2) methane recovery, (3) 1-hour rescuer, (4) use of diesels underground, (5) coal preparation, and (6) manpower development in coal mining.

  1. TiO{sub 2} thin films with rutile phase prepared by DC magnetron co-sputtering at room temperature: Effect of Cu incorporation

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Hui [Institute of Nanoscience and Nanotechnology, College of Physical Science and Technology, Central China Normal University, Wuhan 430079 (China); Hubei Province Key Laboratory of Systems Science in Metallurgical Process, Wuhan University of Science and Technology, Wuhan 430081 (China); Li, Yujie; Ba, Xin; Huang, Lin [Institute of Nanoscience and Nanotechnology, College of Physical Science and Technology, Central China Normal University, Wuhan 430079 (China); Yu, Ying, E-mail: yuying01@mail.ccnu.edu.cn [Institute of Nanoscience and Nanotechnology, College of Physical Science and Technology, Central China Normal University, Wuhan 430079 (China)

    2015-08-01

    Highlights: • TiO{sub 2} film mainly with rutile phase can be prepared by DC sputtering at room temperature with incorporated Cu of modest concentration. • With the increase of Cu-incorporated concentration, the optical band gap of TiO{sub 2} film displays a systematic decrease. • The possible incorporation of Cu{sup 1+} in sites previously occupied by Ti{sup 4+} leads to a gradual change from anatase to rutile phase. - Abstract: The thin films for pure TiO{sub 2} and that incorporated with Cu ion were deposited by DC magnetron co-sputtering with Ar gas. The crystal texture, surface morphology, energy gap and optical properties of the prepared films have been investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectrometer (XPS), UV–vis spectrophotometer, and Raman spectroscopy. The results show that as-deposited TiO{sub 2} film mainly possesses anatase structure at room temperature with pure Ar gas, but the introduction of Cu can alter the phase structure of crystallite TiO{sub 2}. XRD patterns and Raman spectra indicate that the Cu incorporation with high concentration (A{sub Cu}/A{sub Ti} + A{sub Cu} ≈ 20%) favors the formation of rutile phase. Moreover, the Cu incorporation into TiO{sub 2} lattice induces band gap narrowing. Band structures and density of states have been analyzed based on density functional theory (DFT) and periodic models in order to investigate the influence of the Cu incorporation on the electronic structure of TiO{sub 2}. Both experimental data and electronic structure calculations evidence the fact that the change in film structure from the anatase to the rutile phase can be ascribed to the possible incorporation of Cu{sup 1+} in the sites previously occupied by Ti{sup 4+}, and the presence of Cu results in important effect on the electronic states, which is mainly related to the 3d Cu orbitals in the gap and in the vicinity of the valence band edges for TiO{sub 2}.

  2. Preparation of perpendicular oriented TiO2 films via hydrothermal method: phase selection and growth control

    Science.gov (United States)

    Gao, Yun; Guo, Meilan; Xia, Xiaohong; Shao, Guosheng

    2013-03-01

    Either rutile or anatase vertical orientated TiO2 array films were synthesized successfully on FTO (F: SnO2) substrate via hydrothermal method through controlling the concentration of Cl- and SO42- . The density of nanorods can be adjusted by varying the volume ratio of ethanol/water, and the degree of orientation and crystallinity of TiO2 nanofilms were enhanced with increasing dosage of ethanol. Meanwhile, completely dense anatase films with [004] oriented growth appear within a very narrow concentration window when adding sulfuric acid into precursor. Besides, other alcohols such as methanol, n-propanol and n-butyl were also used as solvent to examine the role of alcohol type during hydrothermal process for both two phase films. The growth rate and degree of perpendicular orientation declined as the alkyl length of solvents increases. Hydrogen sensing characteristics of dense films of both rutile and anatase phases showed that there was a remarkable improvement of sensitivity response over reported data. It was found that rutile films have higher sensitivity while anatase films have faster response. This work is supported by Ministry of Education of China (211108) and Science and Technology of Wuhan (2010CDA024, 201110821251).

  3. Characterization and photocatalytic activity of boron-doped TiO2 thin films prepared by liquid phase deposition technique

    Indian Academy of Sciences (India)

    Noor Shahina Begum; H M Farveez Ahmed; O M Hussain

    2008-10-01

    Boron doped TiO2 thin films have been successfully deposited on glass substrate and silicon wafer at 30°C from an aqueous solution of ammonium hexa-fluoro titanate and boron trifluoride by liquid phase deposition technique. The boric acid was used as an – scavenger. The resultant films were characterized by XRD, EDAX, UV and microstructures by SEM. The result shows the deposited film to be amorphous which becomes crystalline between 400 and 500°C. The EDAX and XRD data confirm the existence of boron atom in TiO2 matrix and a small peak corresponding to rutile phase was also found. Boron doped TiO2 thin films can be used as photocatalyst for the photodegradation of chlorobenzene which is a great environmental hazard. It was found that chlorobenzene undergoes degradation efficiently in presence of boron doped TiO2 thin films by exposing its aqueous solution to visible light. The photocatalytic activity increases with increase in the concentration of boron.

  4. Production of dry Lactobacillus rhamnosus GG preparations by spray drying and lyophilization in aqueous two-phase systems

    Directory of Open Access Journals (Sweden)

    Katarzyna Leja

    2009-12-01

    Full Text Available Background. Drying is the oldest method of food preservation. It works by removing water from the food, which prevents the growth of microorganisms and decay. Moreover, spray or freeze drying is also used for the preservation of probiotic cultures. The aim of this study was to compare a survival rate of probiotic bacteria Lactobacillus rhamnosus during spray and freeze drying in ATPS. These results were also compared with survival rate of cells dried under the same conditions but suspended only in skim milk, 6% solution of PVP or 6% solution of dextran. Material and methods. The bacteria Lactobacillus rhamnosus GGwere suspended and spray or freeze dried in various types of aqueous two-phase emulsions: PVP/dextran, PEG4000/dextran and PEG8000/dextran. These emulsions consisted of different types of polymers and had varying ratio of polymers in dispersed (dextran and dispersing (PEG and PVP phases. Results. The research demonstrated that survival rate of bacteria directly after drying depended mainly on protective reagent, rather than on drying method. After 30-day-storage of the dried bacteria cell specimens, the highest survival rate was noted in case of freeze dried cells in milk. In case of spray drying the highest cell survival rate was observed when emulsion PVP3.6%/dextran2.4% was used as a drying medium. Conclusions. Finally, it has been found that cell survival rate was not strongly influenced by the storage temperature of the powder but it depended on the drying medium.  

  5. Highly flexible TiO2-coated stainless steel fabric electrode prepared by liquid-phase deposition

    Science.gov (United States)

    Hwang, Hong Seo; Lee, Jeong Beom; Jung, Jiwon; Lee, Seyoung; Ryu, Ji Heon; Oh, Seung M.

    2016-10-01

    In order to construct flexible lithium-ion batteries, stainless steel (SUS) fabric is used as a current collector for the negative electrode of lithium-ion batteries. TiO2 is coated onto the SUS fabric by liquid-phase deposition to construct an electrode consisting of an SUS wire core and a TiO2 shell. A folding test is then conducted to assess the robustness of TiO2-coated SUS fabric, during which no detachment of TiO2 particles from the SUS current collector is observed; the negative electrode shows a consistent electrochemical cycle performance even under severe physical duress. The TiO2-SUS fabric integration shows excellent flexibility without loss of electrochemical efficacy under mechanical stress, which occurs owing to three main factors. First, the mechanical stress imposed by folding is effectively dissipated by the 3-dimensional structure of the SUS fabric. Secondly, the TiO2 electrode itself is free from mechanical stress owing to negligible volume change during electrochemical cycling. Thirdly, the high interfacial adhesion strength between TiO2 and SUS fabric due to covalent bond formation during liquid-phase deposition prevents the loss of active material from the negative electrode during the folding tests.

  6. Phenylboronic acid modified solid-phase extraction column: Preparation, characterization, and application to the analysis of amino acids in sepia capsule by removing the maltose.

    Science.gov (United States)

    Guo, Mengzhe; Yin, Dengyang; Han, Jie; Zhang, Liyan; Li, Xiao; He, Dandan; Du, Yan; Tang, Daoquan

    2016-09-01

    Maltose, a common auxiliary material of pharmaceutical preparation, may disturb the analysis of total amino acids in sepia capsule by aldolization. Therefore, it is necessary to remove the maltose through a convenient method. In this work, a phenylboronic acid modified solid-phase extraction column has been synthesized and used to remove the maltose. The materials were synthesized by one step "thiol-ene" reaction and the parameters of the column such as absorption capacity, recovery, and absorption specificity have been investigated. The results showed the column (0.5 cm of length × 0.5 cm of inner diameter) can absorb 4.6 mg maltose with a linear absorption and absorption specificity. Then this technique was applied in the quantification of amino acids in sepia capsule. After the optimization of the method, four kinds of amino acids, which were the most abundant, were quantified by high-performance liquid chromatography with diode array detection. The amounts of the four kinds of amino acids are 1.5∼2 times more than that without the treatment of solid-phase extraction column, which almost overcomes the influence of the maltose. All the results indicate that the phenylboronic acid modified solid-phase extraction column can successfully help to accurately quantify the total amino acids in sepia capsule.

  7. Preparation and characterization of silica monolith modified with bovine serum albumin-gold nanoparticles conjugates and its use as chiral stationary phases for capillary electrochromatography.

    Science.gov (United States)

    Lu, Junyu; Ye, Fanggui; Zhang, Aizhu; Wei, Zong; Peng, Yan; Zhao, Shulin

    2011-08-01

    This paper describes the development of silica monolith modified with bovine serum albumin-gold nanoparticles (BSA-GNPs) conjugates as chiral stationary phases for capillary electrochromatography (CEC). The bare monolithic silica column was prepared by a sol-gel process and has been modified chemically with 3-mercaptopropyltrimethoxysilane to provide thiol groups, followed by immobilization of gold nanoparticles via the formation of an Au-S bond and modification with BSA as the chiral selector via the nitrogen lone pair of electrons. It has been demonstrated that the monolithic chiral stationary phases can be used for the enantioseparation of a number of phenylthiocarbamyl amino acids (PTC-D/L-AAs) by CEC. Ten pairs of tested amino acids enantiomers were successfully resolved within 18 min under optimized conditions, and the resolution values were in the range of 1.486-2.083. With PTC-D/L-tryptophan used as the probe solute, the influences of applied voltage, organic modifier and buffer pH in mobile phase on apparent retention factor, enantioselectivity and resolution factor were also investigated.

  8. Phase Composition of Ni/Mg1−xNixO as a Catalyst Prepared for Selective Methanation of CO in H2-Rich Gas

    Directory of Open Access Journals (Sweden)

    Mengmeng Zhang

    2015-01-01

    Full Text Available Supported Ni catalysts Ni/Mg1−xNixO were prepared by reducing samples NiO-MgO in H2/N2 mixture gas at 500°C~800°C for selective methanation of CO in H2-rich gas (CO-SMET. The samples NiO-MgO were obtained by heating water slurry of MgO and Ni(NO32 in a rotary evaporator at 80°C and a final calcination in air at 400°C~800°C. X-ray diffraction (XRD and temperature programmed reduction (TPR measurements demonstrate that the samples NiO-MgO were composed of solid solution Mg1−yNiyO as the main phase and a minor amount of NiO at calcination temperature of 400°C, and amount of the NiO was decreased as calcination temperature increased. Phase composition of the catalysts Ni/Mg1−xNixO was estimated by the Rietveld method. Effects of reduction temperature, feed Ni/Mg ratio, and calcination temperature on phase composition and catalytic activity of the catalysts were investigated. It is clear that CO conversion was generally enhanced by an increased amount of metallic Ni of the catalysts.

  9. Preparation and evaluation of a novel molecularly imprinted polymer coating for selective extraction of indomethacin from biological samples by electrochemically controlled in-tube solid phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Asiabi, Hamid [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah, E-mail: yyamini@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Seidi, Shahram; Ghahramanifard, Fazel [Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran (Iran, Islamic Republic of)

    2016-03-24

    In the present work, an automated on-line electrochemically controlled in-tube solid-phase microextraction (EC-in-tube SPME) coupled with HPLC-UV was developed for the selective extraction and preconcentration of indomethacin as a model analyte in biological samples. Applying an electrical potential can improve the extraction efficiency and provide more convenient manipulation of different properties of the extraction system including selectivity, clean-up, rate, and efficiency. For more enhancement of the selectivity and applicability of this method, a novel molecularly imprinted polymer coated tube was prepared and applied for extraction of indomethacin. For this purpose, nanostructured copolymer coating consisting of polypyrrole doped with ethylene glycol dimethacrylate was prepared on the inner surface of a stainless-steel tube by electrochemical synthesis. The characteristics and application of the tubes were investigated. Electron microscopy provided a cross linked porous surface and the average thickness of the MIP coating was 45 μm. Compared with the non-imprinted polymer coated tubes, the special selectivity for indomethacin was discovered with the molecularly imprinted coated tube. Moreover, stable and reproducible responses were obtained without being considerably influenced by interferences commonly existing in biological samples. Under the optimal conditions, the limits of detection were in the range of 0.07–2.0 μg L{sup −1} in different matrices. This method showed good linearity for indomethacin in the range of 0.1–200 μg L{sup −1}, with coefficients of determination better than 0.996. The inter- and intra-assay precisions (RSD%, n = 3) were respectively in the range of 3.5–8.4% and 2.3–7.6% at three concentration levels of 7, 70 and 150 μg L{sup −1}. The results showed that the proposed method can be successfully applied for selective analysis of indomethacin in biological samples. - Graphical abstract: An automated on

  10. [Preparation of Coated CMC-Fe0 Using Rheological Phase Reaction Method and Research on Degradation of TCE in Water].

    Science.gov (United States)

    Fan, Wen-jing; Cheng, Yue; Yu, Shu-zhen; Fan, Xiao-feng

    2015-06-01

    The coated nanoscale zero-valent iron (coated CMC-Fe0) was synthesized with cheap and environment friendly CMC as the coating agent using rheological phase reaction. The sample was characterized by means of XRD, SEM, TEM and N2 adsorption-stripping and used to study reductive dechlorination of TCE. The experimental results indicated that the removal rate of TCE was about 100% when the CMC-Fe0 dosage was 6 g x L(-1), the initial TCE concentration was 5 mg x L(-1) and the reaction time was 40 h. The TCE degradation reaction of coated CMC-Fe0 followed a pseudo-first-order kinetic model. Finally, the product could be simply recovered.

  11. Preparation and characterization of metal-organic framework MIL-101(Cr)-coated solid-phase microextraction fiber.

    Science.gov (United States)

    Xie, Lijun; Liu, Shuqin; Han, Zhubing; Jiang, Ruifen; Liu, Hong; Zhu, Fang; Zeng, Feng; Su, Chengyong; Ouyang, Gangfeng

    2015-01-01

    Metal-organic frameworks (MOFs) have received great attention as novel sorbents due to their fascinating structures and intriguing potential applications in various fields. In this work, a MIL-101(Cr)-coated solid-phase microextraction (SPME) fiber was fabricated by a simple direct coating method and applied to the determination of volatile compounds (BTEX, benzene, toluene, ethylbenzene, m-xylene and o-xylene) and semi-volatile compounds (PAHs, polycyclic aromatic hydrocarbons) from water samples. The extraction and desorption conditions of headspace SPME (HS-SPME) were optimized. Under the optimized conditions, the established methods exhibited excellent extraction performance. Good precision (recoveries obtained with the spiked river water samples were in the range of 80.0-113% and 84.8-106% for BTEX and PAHs, respectively, which demonstrated the applicability of the self-made fiber.

  12. Effect of titanium oxide compact layer in dye-sensitized solar cell prepared by liquid-phase deposition

    Science.gov (United States)

    Huang, Jung-Jie; Chiu, Shih-Ping; Wu, Menq-Jion; Hsu, Chun-Fa

    2016-11-01

    In this study, titanium dioxide films were deposited on indium tin oxide glass substrates by liquid-phase deposition (LPD) for application as the compact layer in dye-sensitized solar cells (DSSCs). A deposition solution of ammonium hexafluorotitanate and boric acid was used for TiO2 deposition. Compact layer passivation can improve DSSC performance by decreasing carrier losses from recombination at the ITO/electrolyte interface and improving the electrical contact between the ITO and the TiO2 photo-electrode. The optimum thickness of the compact layer was found to be 48 nm, which resulted in a 50 % increase in the conversion efficiency compared with cells without compact layers. The conversion efficiency can be increased from 3.55 to 5.26 %. Therefore, the LPD-TiO2 compact layer inhibits the dark current and increases the short-circuit current density effectively.

  13. ZnO/Cu(InGa)Se.sub.2 solar cells prepared by vapor phase Zn doping

    Science.gov (United States)

    Ramanathan, Kannan; Hasoon, Falah S.; Asher, Sarah E.; Dolan, James; Keane, James C.

    2007-02-20

    A process for making a thin film ZnO/Cu(InGa)Se.sub.2 solar cell without depositing a buffer layer and by Zn doping from a vapor phase, comprising: depositing Cu(InGa)Se.sub.2 layer on a metal back contact deposited on a glass substrate; heating the Cu(InGa)Se.sub.2 layer on the metal back contact on the glass substrate to a temperature range between about 100.degree. C. to about 250.degree. C.; subjecting the heated layer of Cu(InGa)Se.sub.2 to an evaporant species from a Zn compound; and sputter depositing ZnO on the Zn compound evaporant species treated layer of Cu(InGa)Se.sub.2.

  14. Aqueous-Phase Preparation of Model HDS Catalysts on Planar Alumina Substrates: Support Effect on Mo Adsorption and Sulfidation.

    Science.gov (United States)

    Bara, Cédric; Plais, Lucie; Larmier, Kim; Devers, Elodie; Digne, Mathieu; Lamic-Humblot, Anne-Félicie; Pirngruber, Gerhard D; Carrier, Xavier

    2015-12-23

    The role of the oxide support on the structure of the MoS2 active phase (size, morphology, orientation, sulfidation ratio, etc.) remains an open question in hydrotreating catalysis and biomass processing with important industrial implications for the design of improved catalytic formulations. The present work builds on an aqueous-phase surface-science approach using four well-defined α-alumina single crystal surfaces (C (0001), A (112̅0), M (101̅0), and R (11̅02) planes) as surrogates for γ-alumina (the industrial support) in order to discriminate the specific role of individual support facets. The reactivity of the various surface orientations toward molybdenum adsorption is controlled by the speciation of surface hydroxyls that determines the surface charge at the oxide/water interface. The C (0001) plane is inert, and the R (11̅02) plane has a limited Mo adsorption capacity while the A (112̅0) and M (101̅0) surfaces are highly reactive. Sulfidation of model catalysts reveals the highest sulfidation degree for the A (112̅0) and M (101̅0) planes suggesting weak metal/support interactions. Conversely, a low sulfidation rate and shorter MoS2 slabs are found for the R (11̅02) plane implying stronger Mo-O-Al bonds. These limiting cases are reminiscent of type I/type II MoS2 nanostructures. Structural analogies between α- and γ- alumina surfaces allow us to bridge the material gap with real Al2O3-supported catalysts. Hence, it can be proposed that Mo distribution and sulfidation rate are heterogeneous and surface-dependent on industrial γ-Al2O3-supported high-surface-area catalysts. These results demonstrate that a proper control of the γ-alumina morphology is a strategic lever for a molecular-scale design of hydrotreating catalysts.

  15. Differential scanning calorimetry studies on sunscreen loaded solid lipid nanoparticles prepared by the phase inversion temperature method.

    Science.gov (United States)

    Montenegro, L; Sarpietro, M G; Ottimo, S; Puglisi, G; Castelli, F

    2011-08-30

    Solid lipid nanoparticles (SLN) are regarded as interesting carriers to improve sunscreens' safety and effectiveness. In this work, surfactant effects on the physico-chemical properties of SLN loading two of the most widely used UV-filters, octylmethoxycinnamate (OMC) and butylmethoxydibenzoylmethane (BMBM), were evaluated and the interactions between SLN components and loaded UV-filters were investigated by differential scanning calorimetry (DSC). All the SLN showed a mean size ranging from 30 to 95 nm, and a single peak in size distribution. The use of isoceth-20 or oleth-20 as primary surfactants did not provide SLN with suitable physico-chemical properties since: (a) OMC loaded SLN proved unstable; (b) BMBM could not be loaded. OMC or BMBM loaded SLN prepared using ceteth-20 as primary surfactant were stable but their loading capacity lowered when both sunscreens were loaded simultaneously. DSC analyses showed that OMC distributed inside the SLN and caused a decrease of the lipid matrix molecules cooperativity while BMBM did not affect SLN calorimetric behaviour. When OMC and BMBM were loaded together into these SLN, an interaction between BMBM and OMC occurred. These results suggest that the interactions between sunscreens and between sunscreens and SLN components deserve further investigation to evaluate their effect on UV-filter-loaded SLN effectiveness. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Preparation and retention mechanism study of graphene and graphene oxide bonded silica microspheres as stationary phases for high performance liquid chromatography.

    Science.gov (United States)

    Zhang, Xiaoqiong; Chen, Sha; Han, Qiang; Ding, Mingyu

    2013-09-13

    Graphene oxide (GO) bonded stationary phase for high performance liquid chromatography (HPLC) was fabricated by coating GO sheets onto aminosilica microspheres via covalent coupling. Graphene (G) functionalized HPLC stationary phase was then prepared through hydrazine reduction of GO bonded silica (GO@SiO2) composite, which was the first example of using graphene as stationary-phase component for HPLC. Effective separations of the tested neutral and polar compounds on both GO@SiO2 and graphene bonded silica (G@SiO2) columns were achieved under the optimal experimental conditions. Compared with commercial C18 column, the different chromatographic performances of GO and graphene bonded columns were ascribed to their unique retention mechanisms. The polyaromatic scaffold of GO and graphene gives π-π stacking property and hydrophobic effect, and other retention mechanisms, such as π-π electron-donor-acceptor (EDA) interaction for the separation of nitroaromatic compounds and hydrogen bonding for hydroxyl and amino compounds, may also be taken into consideration. Experimental results indicated that the mixed-mode retention mechanism can facilitate the separation of analytes with similar hydrophobicity, which is a unique property compared with C18 column. Additionally, G@SiO2 showed higher affinity to aromatic analytes in contrast with GO@SiO2 and its retention mechanism was not consistent with the typical reversed phase behavior. The separation of aromatic compounds on G@SiO2 column relies primarily on the π-π stacking interaction and then the hydrophobicity, while the two interactions have equal shares on GO@SiO2 column.

  17. Pseudo-ternary phase diagrams of aqueous mixtures of Quil A, cholesterol and phospholipid prepared by the lipid-film hydration method.

    Science.gov (United States)

    Demana, Patrick H; Davies, Nigel M; Vosgerau, Uwe; Rades, Thomas

    2004-02-11

    Pseudo-ternary phase diagrams of the polar lipids Quil A, cholesterol (Chol) and phosphatidylcholine (PC) in aqueous mixtures prepared by the lipid film hydration method (where dried lipid film of phospholipids and cholesterol are hydrated by an aqueous solution of Quil A) were investigated in terms of the types of particulate structures formed therein. Negative staining transmission electron microscopy and polarized light microscopy were used to characterize the colloidal and coarse dispersed particles present in the systems. Pseudo-ternary phase diagrams were established for lipid mixtures hydrated in water and in Tris buffer (pH 7.4). The effect of equilibration time was also studied with respect to systems hydrated in water where the samples were stored for 2 months at 4 degrees C. Depending on the mass ratio of Quil A, Chol and PC in the systems, various colloidal particles including ISCOM matrices, liposomes, ring-like micelles and worm-like micelles were observed. Other colloidal particles were also observed as minor structures in the presence of these predominant colloids including helices, layered structures and lamellae (hexagonal pattern of ring-like micelles). In terms of the conditions which appeared to promote the formation of ISCOM matrices, the area of the phase diagrams associated with systems containing these structures increased in the order: hydrated in water/short equilibration period

  18. Determination of neomycin and related substances in pharmaceutical preparations by reversed-phase high performance liquid chromatography with mass spectrometry and charged aerosol detection.

    Science.gov (United States)

    Stypulkowska, K; Blazewicz, A; Fijalek, Z; Warowna-Grzeskiewicz, M; Srebrzynska, K

    2013-03-25

    A new, simple and repeatable liquid chromatographic method with charged aerosol detection (LC-CAD) for determination of neomycin and related substances has been developed. Analysis of neomycin or other aminoglycosides is problematic due to a lack of chromophores. Universal response of CAD enables direct quantification of neomycin and related substances, for which no reference standard are available. Separation was performed on C18 Hypersil(®) Gold aQ column using water, methanol and heptaflurobutyric acid as mobile phase. Under developed chromatographic conditions all impurities were well separated from neomycin B. Peaks identification was evaluated by electrospray ionization mass spectrometry. The proposed method was validated according to ICH guidelines and applied to the content determination of neomycin and related substances in pharmaceutical preparations.

  19. The Effects and Role of Polyvinylpyrrolidone on the Size and Phase Composition of Iron Oxide Nanoparticles Prepared by a Modified Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Marcela F. Silva

    2017-01-01

    Full Text Available Fe2O3 nanoparticles (as maghemite and hematite mixtures were prepared using adapted sol-gel method from a polyvinylpyrrolidone (PVP aqueous solution in various Fe3+ : PVP monomer ratios. Analysis of X-ray diffraction was obtained to evaluate the crystalline state, average crystallite size, and composition of iron oxide phases. The morphology and average nanoparticles size were evaluated by electronic transmission microscopy. Magnetic properties of iron oxide were analyzed at low and room temperatures. Optical characteristics were evaluated by UV-Vis photoacoustic spectroscopy and the Mössbauer spectrum was obtained in order to evaluate subtle changes in the nuclear environment of the iron atoms.

  20. Research on Si-Al based catalysts prepared by complete liquid-phase method for DME synthesis in a slurry reactor

    Science.gov (United States)

    Li, Zhihong; Zuo, Zhijun; Huang, Wei; Xie, Kechang

    2011-01-01

    A series of Si-Al based DME synthesis catalysts were prepared by complete liquid-phase method and characterized by in situ XPS, XRD, N 2 adsorption and NH 3-TPD analyses. Based on the results, the addition of Si could adjust the pore structure and surface acidity of catalyst, exhibiting a strong promoting effect on the CO conversion and DME selectivity. However, when Si/Al ratio is higher, Si would cover active sites and increase the amount of strong acidity sites, causing the reduction in catalytic activity. It was found from in situ XPS characterization that Cu 0 is the active center of methanol synthesis in DME production, and the addition of Si changes the chemical surroundings of active components and weaken the interaction between Cu, Zn and Al, which maybe give rise to the decrease in catalyst stability.

  1. Preparation of a disulfide-linked precipitative soluble support for solution-phase synthesis of trimeric oligodeoxyribonucleotide 3´-(2-chlorophenylphosphate building blocks

    Directory of Open Access Journals (Sweden)

    Amit M. Jabgunde

    2015-09-01

    Full Text Available The preparation of a disulfide-tethered precipitative soluble support and its use for solution-phase synthesis of trimeric oligodeoxyribonucleotide 3´-(2-chlorophenylphosphate building blocks is described. To obtain the building blocks, N-acyl protected 2´-deoxy-5´-O-(4,4´-dimethoxytritylribonucleosides were phosphorylated with bis(benzotriazol-1-yl 2-chlorophenyl phosphate. The “outdated” phosphotriester strategy, based on coupling of PV building blocks in conjunction with quantitative precipitation of the oligodeoxyribonucleotide with MeOH is applied. Subsequent release of the resulting phosphate and base-protected oligodeoxyribonucleotide trimer 3’-pTpdCBzpdGibu-5’ as its 3’-(2-chlorophenyl phosphate was achieved by reductive cleavage of the disulfide bond.

  2. Preparation of a disulfide-linked precipitative soluble support for solution-phase synthesis of trimeric oligodeoxyribonucleotide 3´-(2-chlorophenylphosphate) building blocks

    Science.gov (United States)

    Molina, Alejandro Gimenez; Virta, Pasi; Lönnberg, Harri

    2015-01-01

    Summary The preparation of a disulfide-tethered precipitative soluble support and its use for solution-phase synthesis of trimeric oligodeoxyribonucleotide 3´-(2-chlorophenylphosphate) building blocks is described. To obtain the building blocks, N-acyl protected 2´-deoxy-5´-O-(4,4´-dimethoxytrityl)ribonucleosides were phosphorylated with bis(benzotriazol-1-yl) 2-chlorophenyl phosphate. The “outdated” phosphotriester strategy, based on coupling of PV building blocks in conjunction with quantitative precipitation of the oligodeoxyribonucleotide with MeOH is applied. Subsequent release of the resulting phosphate and base-protected oligodeoxyribonucleotide trimer 3’-pTpdCBzpdGibu-5’ as its 3’-(2-chlorophenyl phosphate) was achieved by reductive cleavage of the disulfide bond. PMID:26664575

  3. Preparation and antibacterial activity of Ag–TiO2 composite film by liquid phase deposition (LPD) method

    Indian Academy of Sciences (India)

    S-Q Sun; B Sun; Wenqin Zhang; D Wang

    2008-02-01

    A liquid phase deposition (LPD) method has been devised for the deposition of Ag–TiO2 thin films on ceramic tiles with glazed surface at a low temperature. The Ag–TiO2 thin films obtained were welladhered, homogenous and coloured by interference of reflected light. The films were characterized by X-ray diffraction and scanning electron microscopy. From these analyses, it was found that silver ions were trapped in TiO2 matrix and their reduction could be achieved at 600°C annealing temperature. The antibacterial activity against S. aureus and . coli has been studied applying the so called antibacterial-drop test. The Ag–TiO2 thin films exhibited a high antibacterial activity. AAS was used for the quantitave determination of silver ion concentration releasing from the Ag–TiO2 thin film. The releasing rate of silver ions from the Ag–TiO2 film was 0.118 g/ml during 192 h. The antibacterial effect of Ag–TiO2 thin film before and after aging in a weathering chamber for 48 h was compared and the results show that the antibacterial activity is not compromised after weathering.

  4. Increasing the thermal storage capacity of a phase change material by encapsulation: preparation and application in natural rubber.

    Science.gov (United States)

    Phadungphatthanakoon, Songpon; Poompradub, Sirilux; Wanichwecharungruang, Supason P

    2011-09-01

    Existing encapsulated organic phase change materials (PCM) usually contain a shell material that possesses a poor heat storage capacity and so results in a lowered latent heat storage density of the encapsulated PCM compared to unencapsulated PCM. Here, we demonstrate the use of a novel microencapsulation process to encapsulate n-eicosane (C20) into a 2:1 (w/w) ratio blend of ethyl cellulose (EC):methyl cellulose (MC) to give C20-loaded EC/MC microspheres with an increased heat storage capacity compared to the unencapsulated C20. Up to a 29 and 24% increase in the absolute enthalpy value during crystallization and melting were observed for the encap-C20/EC/MC microparticles with a 9% (w/w) EC/MC polymer content. The mechanism that leads to the increased latent heat storage capacity is discussed. The blending of the water-dispersible C20-loaded EC/MC microspheres into natural rubber latex showed excellent compatibility, and the obtained rubber composite showed not only an obvious thermoregulation property but also an improved mechanical property.

  5. Recovery Efficiency Test Project: Phase 1, Activity report. Volume 1: Site selection, drill plan preparation, drilling, logging, and coring operations

    Energy Technology Data Exchange (ETDEWEB)

    Overbey, W.K. Jr.; Carden, R.S.; Kirr, J.N.

    1987-04-01

    The recovery Efficiency Test well project addressed a number of technical issues. The primary objective was to determine the increased efficiency gas recovery of a long horizontal wellbore over that of a vertical wellbore and, more specifically, what improvements can be expected from inducing multiple hydraulic fractures from such a wellbore. BDM corporation located, planned, and drilled a long radius turn horizontal well in the Devonian shale Lower Huron section in Wayne County, West Virginia, demonstrating that state-of-the-art technology is capable of drilling such wells. BDM successfully tested drilling, coring, and logging in a horizontal well using air as the circulating medium; conducted reservoir modeling studies to protect flow rates and reserves in advance of drilling operations; observed two phase flow conditions in the wellbore not observed previously; cored a fracture zone which produced gas; observed that fractures in the core and the wellbore were not systematically spaced (varied from 5 to 68 feet in different parts of the wellbore); observed that highest gas show rates reported by the mud logger corresponded to zone with lowest fracture spacing (five feet) or high fracture frequency. Four and one-half inch casting was successfully installed in the borehole and was equipped to isolate the horizontal section into eight (8) zones for future testing and stimulation operations. 6 refs., 48 figs., 10 tabs.

  6. Low-temperature solid state synthesis and in situ phase transformation to prepare nearly pure cBN.

    Science.gov (United States)

    Lian, Gang; Zhang, Xiao; Tan, Miao; Zhang, Shunjie; Cui, Deliang; Wang, Qilong

    2011-07-14

    Cubic boron nitride (cBN) is synthesized by a low-temperature solid state synthesis and in situ phase transformation route with NH(4)BF(4), B, NaBH(4) and KBH(4) as the boron sources and NaN(3) as the nitrogen source. Furthermore, two new strategies are developed, i.e., applying pressure on the reactants during the reaction process and introducing the structural induction effect. These results reveal that the relative contents of cBN are greatly increased by applying these new strategies. Finally, almost pure cBN (∼90%) crystals are obtained by reacting NH(4)BF(4) and NaN(3) at 250 °C and 450 MPa for 24 h, with NaF as the structural induction material. The heterogeneous nucleation mechanism can commendably illuminate the structure induction effect of NaF with face center cubic structure. In addition, the induction effect results in the cBN nanocrystals presenting obvious oriented growth of {111} planes.

  7. Preparation and Characterization of Single-Phase Perovskite La0.6Sr0.4Co0.8Fe0.2O3-δ

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    Single-phase perovskite La0.6Sr0.4Co0.8Fe0.2O3-δ has been successfully prepared by using citrate-EDTA complexation method at relatively low calcination temperature. The structure and thermal decomposition process of the complex precursor have been investigated by means of differential scanning calorimetry-thermal gravimetric analysis (DSC/TGA), X-ray diffraction (XRD), and Fourier transform infrared spectroscopic (FT-IR) measurements. The precursor decomposed completely and started to form perovskite-type oxide above 420 ℃ according to the differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) results. Single-phase perovskite La0.6Sr0.4Co0.8Fe0.2O3-δ obtained has been confirmed from the XRD pattern, and no peak of SrCO3 was found by XRD of the oxides synthesized at a relatively low temperature of 800 ℃. The reducibility of La0.6Sr0.4Co0.8Fe0.2O3-δ was also characterized by the temperature programmed reduction (TPR) technique. Disk shaped dense La0.6Sr0.4Co0.8Fe0.2O3-δ membrane was prepared by the isostatical pressing method. The oxygen flux rate of dense La0.6Sr0.4Co0.8Fe0.2O3-δ membrane was (2.8-18) × 10-8 mol/(cm2.s) in the temperature range of 800-1000 ℃.

  8. Sol-gel preparation of TiO{sub 2}-ZrO{sub 2} thin films supported on glass rings: Influence of phase composition on photocatalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez-Alonso, Maria D. [Instituto de Catalisis y Petroleoquimica, CSIC, c/ Marie Curie, 2. Cantoblanco. 28049 Madrid (Spain)]. E-mail: mdhernandez@icp.csic.es; Tejedor-Tejedor, Isabel [Environmental Chemistry and Technology Program, University of Wisconsin, 660 North Park Street, Madison, WI 53706 (United States); Coronado, Juan M. [Instituto de Catalisis y Petroleoquimica, CSIC, c/ Marie Curie, 2. Cantoblanco. 28049 Madrid (Spain)]. E-mail: juanmanuel.coronado@ciemat.es; Soria, Javier [Instituto de Catalisis y Petroleoquimica, CSIC, c/ Marie Curie, 2. Cantoblanco. 28049 Madrid (Spain); Anderson, Marc A. [Environmental Chemistry and Technology Program, University of Wisconsin, 660 North Park Street, Madison, WI 53706 (United States)

    2006-04-28

    In order to optimize the characteristics of TiO{sub 2}-ZrO{sub 2} thin films supported on glass for the photocatalytic removal of VOCs, acidic sols of different composition (ZrO{sub 2}, TiO{sub 2} and Ti-Zr mixed oxides) have been prepared using metal alkoxides as starting materials. The photoactive oxides were deposited on 'Raschig rings' of borosilicate glass using a dip-coating technique. The phase composition of the thin films was controlled during the sol preparation stage to produce either (1) Ti{sub 0.9}Zr{sub 0.1}O{sub 2} solid solutions, or (2) ZrO{sub 2}/TiO{sub 2} binary metal oxides (10% and 20% molar content of Zr). The particle size of the different sols was measured by photon correlation spectroscopy, and the xerogels were characterized by XRD, N{sub 2} adsorption isotherms, and TG-DTA, so as to monitor the modifications induced by the thermal treatments. Raman spectroscopy was used to determine the crystalline structure of the supported TiO{sub 2}-ZrO{sub 2} oxides, which in all cases corresponded to the anatase phase. The band gap of the thin films was estimated from the UV-vis spectra, and none of them differed significantly from that of unmodified TiO{sub 2}. The photoactivity of the coated glass 'Raschig rings' was measured for the oxidation of acetone and methylcyclohexane vapors using, respectively, total recycle and single pass plug flow photoreactors. The results obtained indicate that, for the same Zr content, the photoactivity of the films containing binary metal oxides is slightly higher than that of the solid solution. In contrast, specific surface area seems to have little influence on the performance of the thin films.

  9. Triterpene-loaded microemulsion using Coix lacryma-jobi seed extract as oil phase for enhanced antitumor efficacy: preparation and in vivo evaluation

    Directory of Open Access Journals (Sweden)

    Qu D

    2013-12-01

    Full Text Available Ding Qu, Junjie He, Congyan Liu, Jing Zhou, Yan ChenKey Laboratory of New Drug Delivery System of Chinese Materia Medica, Jiangsu Provincial Academy of Chinese Medicine, Jiangsu, People’s Republic of ChinaAbstract: Ganoderma lucidum triterpene-loaded microemulsions (TMEs using Coix lacryma-jobi (adlay seed oil as oil phase were prepared, characterized, and evaluated for enhanced antitumor activity. Ternary phase diagrams for the TMEs were constructed and the optimal preparation was developed. Transmission electron microscopy and dynamic light scattering showed that this formulation had a well defined spherical shape, a homogeneous distribution, a small size, and a narrow polydispersity index. The drug-loading rate was determined to be 9.87% by ultraviolet spectrophotometry, and acceptable stability under various stimulations in vitro was confirmed. Importantly, the TME formulation showed a significantly greater antiproliferative effect towards human lung carcinoma (A549 cells and murine lung tumor (Lewis cells in comparison with suspension formulations containing triterpene and adlay seed oil as a positive control. The half-maximal inhibitory concentration of the TMEs was about 0.62 mg crude drug per mL, being 2.5-fold improved relative to that of the corresponding suspension formulation, but no significant cytotoxicity was observed for the bare microemulsion in A549 cells and Lewis cells. In vivo, the TME formulation showed markedly enhanced antitumor efficacy in a xenograft model of Lewis lung cancer after intragastric administration. Compared with cyclophosphamide, the TME formulation showed similar antitumor activity but less general toxicity. These results indicate the feasibility of using a microemulsion to increase the solubility of triterpene and adlay. TMEs hold promise as an efficient drug delivery system for the treatment of lung cancer.Keywords: microemulsion, Ganoderma lucidum, triterpene, adlay seed oil, lung cancer

  10. Facile preparation of protein stationary phase based on polydopamine/graphene oxide platform for chip-based open tubular capillary electrochromatography enantioseparation.

    Science.gov (United States)

    Liang, Ru-Ping; Wang, Xiao-Ni; Liu, Chun-Ming; Meng, Xiang-Ying; Qiu, Jian-Ding

    2014-01-03

    A novel chip-based enantioselective open-tubular capillary electrochromatography (OT-CEC) was developed employing bovine serum albumin (BSA) conjugated polydopamine-graphene oxide (PDA/GO) nanocomposites (PDA/GO/BSA) as stationary phase. After the poly(dimethylsiloxane) (PDMS) microfluidic chip was filled with a freshly prepared solution containing dopamine and graphene oxide, PDA/GO nanocomposites were formed and deposited on the inner wall of microchannel as permanent coating via the oxidation of dopamine by the oxygen dissolved in the solution. The PDA/GO-coated PDMS microchips not only have the adhesion of PDA that make them easily immobilized in the microchannel, but also have the larger surface and excellent biocompatibility of graphene which can incorporate much more biomolecules and well maintain their biological activity. In addition, incorporation of GO in PDA film can make surface morphology more rough, which is beneficial for enhancing the loading capacity of proteins in the microchannels and increasing sample capacity of OT-CEC columns. BSA was stably immobilized in the PDMS microchannel to fabricate a protein-stationary phase. Compared with the native PDMS microchannels, the modified surfaces exhibited much better wettability, more stable electroosmotic mobility, and less nonspecific adsorption. The efficient separation of chiral amino acids (tryptophan and threonine) and chiral dipeptide demonstrate that the constructed OT-CEC columns own ideal enantioselectivity. The presented strategy using PDA/GO coating as a versatile platform for facile conjugation of proteins may offer new processing strategies to prepare a functional surface designed on microfluidic chips. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Development of a Gradient HPLC Method for the Simultaneous Determination of Sotalol and Sorbate in Oral Liquid Preparations Using Solid Core Stationary Phase

    Directory of Open Access Journals (Sweden)

    Ludmila Matysova

    2015-01-01

    Full Text Available A selective and sensitive gradient HPLC-UV method for quantification of sotalol hydrochloride and potassium sorbate in five types of oral liquid preparations was developed and fully validated. The separation of an active substance sotalol hydrochloride, potassium sorbate (antimicrobial agent, and other substances (for taste and smell correction, etc. was performed using an Ascentis Express C18 (100 × 4.6 mm, particles 2.7 μm solid core HPLC column. Linear gradient elution mode with a flow rate of 1.3 mL min−1 was used, and the injection volume was 5 µL. The UV/Vis absorbance detector was set to a wavelength of 237 nm, and the column oven was conditioned at 25°C. A sodium dihydrogen phosphate dihydrate solution (pH 2.5; 17.7 mM was used as the mobile phase buffer. The total analysis time was 4.5 min (+2.5 min for reequilibration. The method was successfully employed in a stability evaluation of the developed formulations, which are now already being used in the therapy of arrhythmias in pediatric patients; the method is also suitable for general quality control, that is, not only just for extemporaneous preparations containing the mentioned substances.

  12. Preparation of sulfonated graphene/polypyrrole solid-phase microextraction coating by in situ electrochemical polymerization for analysis of trace terpenes.

    Science.gov (United States)

    Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

    2014-06-13

    In this study, a novel sulfonated graphene/polypyrrole (SG/PPy) solid-phase microextraction (SPME) coating was prepared and fabricated on a stainless-steel wire by a one-step in situ electrochemical polymerization method. Crucial preparation conditions were optimized as polymerization time of 15min and SG doping amount of 1.5mg/mL. SG/PPy coating showed excellent thermal stability and mechanical durability with a long lifespan of more than 200 stable replicate extractions. SG/PPy coating demonstrated higher extraction selectivity and capacity to volatile terpenes than commonly-used commercial coatings. Finally, SG/PPy coating was practically applied for the analysis of volatile components from star anise and fennel samples. The majority of volatile components identified were terpenes, which suggested the ultra-high extraction selectivity of SG/PPy coating to terpenes during real analytical projects. Four typical volatile terpenes were further quantified to be 0.2-27.4μg/g from star anise samples with good recoveries of 76.4-97.8% and 0.1-1.6μg/g from fennel samples with good recoveries of 80.0-93.1%, respectively.

  13. Preparation of solid-phase microextraction fibers by in-mold coating strategy for derivatization analysis of 24-epibrassinolide in pollen samples.

    Science.gov (United States)

    Pan, Jialiang; Hu, Yuling; Liang, Tingan; Li, Gongke

    2012-11-02

    A novel and simple in-mold coating strategy was proposed for the preparation of uniform solid-phase microextraction (SPME) coatings. Such a strategy is based on the direct synthesis of the polymer coating on the surface of a solid fiber using a glass capillary as the mold. The capillary was removed and the polymer with well-controlled thickness could be coated on the silica fiber reproductively. Following the strategy, a new poly(acrylamide-co-ethylene glycol dimethacrylate) (poly(AM-co-EGDMA)) coating was prepared for the preconcentration of 24-epibrassinolide (24-epiBL) from plant matrix. The coating had the enrichment factor of 32 folds, and the extraction efficiency per unit thickness was 5 times higher than that of the commercial polydimethylsiloxane/divinylbenzene (PDMS/DVB) coating. A novel method based on SPME coupled with derivatization and large volume injection-high performance liquid chromatography (LVI-HPLC) was developed for the analysis of 24-epiBL. The linear range was 0.500-20.0 μg/L with the detection limit of 0.13 μg/L. The amounts of endogenous 24-epiBL in rape and sunflower breaking-wall pollens samples were determined with satisfactory recovery (77.8-104%) and reproducibility (3.9-7.9%). The SPME-DE/LVI-HPLC method is rapid, reliable, convenient and applicable for complicated plant samples.

  14. Green Preparation of Epoxy/Graphene Oxide Nanocomposites Using a Glycidylamine Epoxy Resin as the Surface Modifier and Phase Transfer Agent of Graphene Oxide.

    Science.gov (United States)

    Tang, Xinlei; Zhou, Yang; Peng, Mao

    2016-01-27

    In studies of epoxy/graphene oxide (GO) nanocomposites, organic solvents are commonly used to disperse GO, and vigorous mechanical processes and complicated modification of GO are usually required, increasing the cost and hindering the development and application of epoxy nanocomposites. Here, we report a green, facile, and efficient method of preparing epoxy/GO nanocomposites. When triglycidyl para-aminophenol (TGPAP), a commercially available glycidyl amine epoxy resin with one tertiary amine group per molecule, is used as both the surface modifier and phase transfer agent of GO, GO can be directly and rapidly transferred from water to diglycidyl ether of bisphenol A and other types of epoxy resins by manual stirring under ambient conditions, whereas GO cannot be transferred to these epoxy resins in the absence of TGPAP. The interaction between TGPAP and GO and the effect of the TGPAP content on the dispersion of GO in the epoxy matrix were investigated systematically. Superior dispersion and exfoliation of GO nanosheets and remarkably improved mechanical properties, including tensile and flexural properties, toughness, storage modulus, and microhardness, of the epoxy/GO nanocomposites with a suitable amount of TGPAP were demonstrated. This method is organic-solvent-free and technically feasible for large-scale preparation of high-performance nanocomposites; it opens up new opportunities for exploiting the unique properties of graphene or even other nanofillers for a wide range of applications.

  15. Preparation and characteristics of high pH-resistant sol-gel alumina-based hybrid organic-inorganic coating for solid-phase microextraction of polar compounds.

    Science.gov (United States)

    Liu, Mingming; Liu, Ying; Zeng, Zhaorui; Peng, Tianyou

    2006-03-10

    A novel alumina-based hybrid organic-inorganic sol-gel coating was first developed for solid-phase microextraction (SPME) from a highly reactive alkoxide precursor, aluminum sec-butoxide, and a sol-gel-active organic polymer hydroxyl-terminated polydimethylsiloxane (OH-TSO). The underlying mechanism was discussed and confirmed by IR spectra. The porous surface structure of the sol-gel coating was revealed by scanning electron microscopy. A detailed investigation was conducted to evaluate the remarked performance of the newly developed sol-gel alumina-OH-TSO hybrid materials. In stark contrast to the sol-gel silica-based coating, the alumina-based coating demonstrated excellent pH stability. In addition, good thermal resistance and coating preparation reproducibility are also its outstanding performance. As compared to silica-based hybrids material, the ligand exchange ability of alumina makes it structurally superior extraction sorbents for polar compounds, such as fatty acids, phenols, alcohols, aldehydes and amines. Practical applicability of the prepared alumina-OH-TSO fiber was demonstrated through the analysis of volatile alcohols and fatty acids in beer. The recoveries obtained ranged from 85.7 to 104% and the relative standard deviation values for all analytes were below 9%.

  16. Preparation of an additive-free sample with a MgH2 phase by planetary ball milling of Mg with10 wt% MgH2

    Science.gov (United States)

    Hong, Seong-Hyeon; Song, Myoung Youp

    2016-11-01

    In order to prepare an additive-free sample with a MgH2 phase, 90 wt% Mg+10 wt% MgH2 (named Mg-10MgH2) was milled under hydrogen atmosphere in a planetary ball mill for different durations (2 h, 5 h, and 10 h). The hydrogen absorption and release properties of the prepared samples were investigated and compared with those of purchased pure MgH2 samples. Mg-10MgH2 milled for 5 h had the largest quantity of hydrogen released at 648 K for 100 min of 5.96 wt%. Mg-10MgH2 milled for 5 h released 0.11 wt% H for 10 min, 4.85 wt% H for 30 min, and 5.83 wt% H for 60 min at 648 K at the first cycle. Mg-10MgH2 milled for 5 h absorbed 5.39 wt% H for 5 min and 5.92 wt% H for 60 min at 648 K at the second cycle. Dehydriding curves were also obtained at the first cycle of Mg-10MgH2 samples milled for 5 h using Mg powder with or without sieving (200 mesh). The dehydriding curve at 648 K of a Mg-10MgH2 sample milled for 5 h in the planetary ball mill was compared with that of the sample milled for 24 h in a horizontal ball mill.

  17. Preparation, characterization and thermal properties of styrene maleic anhydride copolymer (SMA)/fatty acid composites as form stable phase change materials

    Energy Technology Data Exchange (ETDEWEB)

    Sari, Ahmet; Alkan, Cemil; Karaipekli, Ali; Oenal, Adem [Department of Chemistry, Gaziosmanpasa University, 60240, Tokat (Turkey)

    2008-02-15

    Fatty acids such as stearic acid (SA), palmitic acid (PA), myristic acid (MA) and lauric acid (LA) are promising phase change materials (PCMs) for latent heat thermal energy storage (LHTES) applications, but high cost is the major drawback of them, limiting their utility area in thermal energy storage. The use of fatty acids as form stable PCMs will increase their feasibilities in practical applications due to the reduced cost of the LHTES system. In this regard, a series of styrene maleic anhydride copolymer (SMA)/fatty acid composites, SMA/SA, SMA/PA, SMA/MA, and SMA/LA, were prepared as form stable PCMs by encapsulation of fatty acids into the SMA, which acts as a supporting material. The encapsulation ratio of fatty acids was as much as 85 wt.% and no leakage of fatty acid was observed even when the temperature of the form stable PCM was over the melting point of the fatty acid in the composite. The prepared form stable composite PCMs were characterized using optic microscopy (OM), viscosimetry and Fourier transform infrared (FT-IR) spectroscopy methods, and the results showed that the SMA was physically and chemically compatible with the fatty acids. In addition, the thermal characteristics such as melting and freezing temperatures and latent heats of the form stable composite PCMs were measured by using the differential scanning calorimetry (DSC) technique, which indicated they had good thermal properties. On the basis of all the results, it was concluded that form stable SMA/fatty acid composite PCMs had important potential for practical LHTES applications such as under floor space heating of buildings and passive solar space heating of buildings by using wallboard, plasterboard or floors impregnated with a form stable PCM due to their satisfying thermal properties, easy preparation in desired dimensions, direct usability without needing additional encapsulation thereby eliminating the thermal resistance caused by the shell and, thus, reducing the cost of

  18. Preparation and properties of 1-tetradecanol/1,3:2,4-di-(3,4-dimethyl) benzylidene sorbitol gelatinous form-stable phase change materials

    Energy Technology Data Exchange (ETDEWEB)

    Tian, Tuo; Song, Jian; Niu, Libo [School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Feng, Rongxiu, E-mail: rxfeng7091@tju.edu.cn [School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China)

    2013-02-20

    Graphical abstract: The 1,3:2,4-di-(3,4-dimethyl) benzylidene sorbitol can self-assemble to form three-dimensional network and immobilized the 1-tetradecanol. As a result, the gel-to-sol transition temperature of the composite PCM increased and the 1-tetradecanol leakage decreased. Highlights: ► First used of 1,3:2,4-di-(3,4-dimethyl) benzylidene sorbitol in alcohol-based PCMs. ► A new method of doping with exfoliated graphite is presented. ► A possible mechanism for decreasing leakage has been proposed based on SEM results. ► The prepared composite PCMs showed a high-energy storage density. ► The addition of exfoliated graphite enhanced the thermal conductivity of the PCMs. - Abstract: A 1-tetradecanol (TD)/1,3:2,4-di-(3,4-dimethyl) benzylidene sorbitol (DMDBS) composite was prepared as a novel form-stable phase change material (PCM), and the properties of the composites such as the gel-to-sol transition temperature, the latent heat, the microstructure and the thermal storage performance were characterized. The composite was prepared by impregnating DMDBS into TD and the maximum feasible weight percentage of TD was determined to be 94.2 wt%. The gel-to-sol transition temperature of the composite PCM was 158.3–180.0 °C, which is well above the melting point of 1-tetradecanol. Differential scanning calorimeter (DSC) was used to determine the melting and freezing enthalpies of 1-tetradecanol in the composite PCM and the values are 218.5 and 215.3 J g{sup −1}, respectively. Scanning electron microscopy (SEM) results showed that 1-tetradecanol dispersed in the three-dimensional network formed by DMDBS. The relationship between the amount of DMDBS additive and the leakage was also discussed. The thermal conductivity of the composite PCM was improved by doping with exfoliated graphite.

  19. Preparation of AgInS₂ quantum dot/In₂S₃ co-sensitized photoelectrodes by a facile aqueous-phase synthesis route and their photovoltaic performance.

    Science.gov (United States)

    Wang, Yuanqiang; Zhang, Qinghong; Li, Yaogang; Wang, Hongzhi

    2015-04-14

    In an aqueous-phase system, AgInS2 quantum dot (QD) sensitized TiO2 photoanodes were prepared in situ by the reaction of β-In2S3 nanocrystals and as-prepared TiO2/Ag2S-QD electrodes, followed by a covering process with a ZnS passivation layer. A facile successive ionic layer adsorption and reaction (SILAR) method was adopted to obtain TiO2/Ag2S-QD electrodes. β-In2S3 nanocrystals synthesized by the chemical bath deposition (CBD) process serve as the reactant of AgInS2 as well as a buffer layer between the interfaces of TiO2 and AgInS2-QDs. A polysulfide electrolyte and a Pt-coated FTO glass count electrode were used to test the photovoltaic performance of the constructed devices. The characteristics of the sensitized photoelectrodes were studied in more detail by electron microscopy, X-ray techniques, and optical and photoelectric performance measurements. AgInS2 is the main photo-sensitizer for TiO2/AgInS2-QD/In2S3 electrodes and excess In2S3 appears on the surface of the electrodes. Based on the optimal Ag2S SILAR cycle, the best photovoltaic performance of the prepared TiO2/AgInS2-QD/In2S3 electrode with the short-circuit photocurrent density (Jsc) of 7.87 mA cm(-2) and power conversion efficiency (η) of 0.70% under full one-sun illumination was achieved.

  20. [Preparation of molecularly imprinted polymers using dummy template and the applications in selective solid-phase extraction of seven bisphenols from human urine, bovine serum and beer samples].

    Science.gov (United States)

    Yang, Jiajia; Li, Yun; Wang Jinchengt; Sun, Xiaoli; Chen, Jiping

    2015-05-01

    A molecularly imprinted polymer (MIP) for selective recognition of seven bisphenols (BPs) was prepared using dummy template phenolphthalein (PP) by bulk polymerization. The characterization results of scanning electron microscopy and nitrogen adsorption-desorption measurements showed that the prepared PP-MIP possessed narrow particle diameter distribution (40-60 µm), a specific surface area (S(BET)) of 359.77 m2/g and a total pore volume (Vt) of 0.730 cm3/g. The adsorption capacity for bisphenol A (BPA) of PP-MIP was evaluated by static adsorption experiment. And the Scatchard analysis revealed that the maximum specific adsorption capacity of PP-MIP was 4.661 µmol/g. Good class selectivity for BPA and its six structural analogues of bisphenol B (BPB) , bisphenol E (BPE), bisphenol AF (BPAF), bisphenol S (BPS), bisphenol AP (BPAP) and bisphenol Z (BPZ) was demonstrated by the chromatographic evaluation experiment. The prepared PP-MIP was successfully used as solid-phase extraction (SPE) sorbent for the separation and purification of the seven BPs in human urine, bovine serum and beer samples. Meanwhile, an accurate and sensitive MIP-SPE-HPLC method was established for the determination of the seven BPs in human urine, bovine serum and beer samples. The limits of detection (LODs) for the three samples were in the range of 1.2-2.0 µg/L. The results showed that good linearities were obtained in the range of 0.02-2 mg/L for the seven BPs and the correlation coefficients (r) were higher than 0.999 8. The recoveries of the BPs spiked in blank samples at two spiked levels (100 and 500 µg/L for each BP) were in the range of 90.1%-107.1% with the RSDs ≤ 8.1%. The proposed method is simple and reliable for the rapid detection of the seven BPs in human urine, bovine serum and beer samples.

  1. Facile and fast preparation of low-cost silica-supported graphitic carbon nitride for solid-phase extraction of fluoroquinolone drugs from environmental waters.

    Science.gov (United States)

    Speltini, Andrea; Maraschi, Federica; Govoni, Roberta; Milanese, Chiara; Profumo, Antonella; Malavasi, Lorenzo; Sturini, Michela

    2017-03-17

    The analytical application of silica-supported graphitic carbon nitride (g-C3N4@silica) for solid-phase extraction (SPE) of fluoroquinolone (FQ) pollutants from water is presented for the first time. g-C3N4@silica was easily and quickly prepared by one-pot thermal condensation of dicyandiamide and characterized by powder X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, Fourier transform infrared spectroscopy and surface area measurements. The novel composite was applied as sorbent for SPE of FQs from water prior high-performance liquid chromatography with fluorescence detection. The extraction efficiency of g-C3N4 was tested in tap and surface waters at actual concentrations (10-100ngL(-1)). Quantitative adsorption was achieved using 100mg sorbent (20wt% g-C3N4) for pre-concentration of 50-500mL sample, at the native pH (∼7.5-8). Elution was performed with 25mM H3PO4 aqueous solution-acetonitrile (80:20), obtaining recoveries in the range 70-114%, enrichment factors up to 500 and inter-day RSDs≤12%. The batch-to-batch reproducibility was assessed on three independently synthesized g-C3N4@silica preparations (RSD 6-12%). g-C3N4 supported on silica microparticles proved to be of easy preparation, inexpensive, reusable for at least 4 extractions of raw surface waters, and suitable for determination in real matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Combination of dispersive liquid-liquid microextraction and solid-phase microextraction: An efficient hyphenated sample preparation method.

    Science.gov (United States)

    Jafari, Mohammad T; Saraji, Mohammad; Mossaddegh, Mehdi

    2016-09-30

    Two well-known microextraction methods, dispersive liquid-liquid microextraction (DLLME) and solid-phase microextraction (SPME), were combined, resulting in as an encouraging method. The method, named DLLME-SPME, was performed based on total vaporization technique. For the DLLME step, 1,1,2,2-tetrachloroethane and acetonitrile were used as extraction and disperser solvents, respectively. Halloysite nanotubes-titanium dioxide was used as the fiber coating in the SPME step. The method was applied for the extraction of diazinon and parathion (as the test compounds) in environmental water samples and fruit juices, and gas chromatography-corona discharge ion mobility spectrometry was used as the determination apparatus. Desorption temperature and time, extraction temperature and time, and the volume of the extracting solvent in the DLLME step were optimized as the effective parameters on the extraction efficiency. The relative standard deviations (RSDs) of intra-day were found to be 4-7% and 6-8% for diazinon and parathion, respectively. Also, the RSDs of inter-day were 7-9% and 8-10% for diazinon and parathion, respectively. The limits of quantification and detection were obtained to be 0.015 and 0.005μgL(-1) for diazinon, and 0.020 and 0.007μgL(-1) for parathion. A good linearity range (r(2)˃0.993) was obtained in the range of 0.015-3.000 and 0.020-3.000μgL(-1) for diazinon and parathion, respectively. The high enrichment factors were obtained as 3150 and 2965 for diazinon and parathion, respectively. This method showed high sensitivity with good recovery values (between 87 and 99%) for the extraction of target analytes in the real samples. Overall, the results revealed that the developed DLLME-SPME method had better extraction efficiency than DLLME and SPME alone.

  3. Fluoride adsorption studies on mixed-phase nano iron oxides prepared by surfactant mediation-precipitation technique

    Energy Technology Data Exchange (ETDEWEB)

    Mohapatra, M., E-mail: mamatamohapatra@yahoo.com [Institute of Minerals and Materials Technology, Acharyavihar, Bhubaneswar 751 013, Orissa (India); Rout, K. [Institute of Minerals and Materials Technology, Acharyavihar, Bhubaneswar 751 013, Orissa (India); Singh, P. [Murdoch University, Perth, Western Australia (Australia); Anand, S. [Institute of Minerals and Materials Technology, Acharyavihar, Bhubaneswar 751 013, Orissa (India); Layek, S.; Verma, H.C. [Indian Institute of Technology, Kanpur (India); Mishra, B.K. [Institute of Minerals and Materials Technology, Acharyavihar, Bhubaneswar 751 013, Orissa (India)

    2011-02-28

    Mixed nano iron oxides powder containing goethite ({alpha}-FeOOH), hematite ({alpha}-Fe{sub 2}O{sub 3}) and ferrihydrite (Fe{sub 5}HO{sub 8}.4H{sub 2}O) was synthesized through surfactant mediation-precipitation route using cetyltrimethyl ammonium bromide (CTAB). The X-ray diffraction, FTIR, TEM, Moessbauer spectroscopy were employed to characterize the sample. These studies confirmed the nano powder contained 77% goethite, 9% hematite and 14% ferrihydrite. Fluoride adsorption onto the synthesized sample was investigated using batch adsorption method. The experimental parameters chosen for adsorption studies were: pH (3.0-10.0), temperature (35-55 deg. C), concentrations of adsorbent (0.5-3.0 g/L), adsorbate (10-100 mg/L) and some anions. Adsorption of fluoride onto mixed iron oxide was initially very fast followed by a slow adsorption phase. By varying the initial pH in the range of 3.0-10.0, maximum adsorption was observed at a pH of 5.75. Presence of either SO{sub 4}{sup 2-} or Cl{sup -} adversely affected the adsorption of fluoride in the order of SO{sub 4}{sup 2-} > Cl{sup -}. The FTIR studies of fluoride loaded adsorbent showed that partly the adsorption on the surface took place at surface hydroxyl sites. Moessbauer studies indicated that the overall absorption had gone down after fluoride adsorption that implies it has reduced the crystalline bond strength. The relative absorption area of ferrihydrite was marginally increased from 14 to 17%.

  4. Physical and electrochemical characterization of CdS hollow microspheres prepared by a novel template free solution phase method

    Energy Technology Data Exchange (ETDEWEB)

    Rengaraj, S., E-mail: rengaraj.selvaraj@uef.f [University of Eastern Finland, Laboratory of Applied Environmental Chemistry (LAEC), Patteristonkatu 1, FI-50100 Mikkeli (Finland); Ferancova, A. [University of Eastern Finland, Laboratory of Applied Environmental Chemistry (LAEC), Patteristonkatu 1, FI-50100 Mikkeli (Finland); Institute of Analytical Chemistry, Slovak University of Technology in Bratislava, 81237 Bratislava (Slovakia); Jee, S.H. [Department of Chemical Engineering, Kwangwoon University, Wolgye, Nowon, Seoul 139-701 (Korea, Republic of); Venkataraj, S. [Crystal Growth Centre, Anna University, Chennai 600025 (India); Kim, Y. [Department of Chemical Engineering, Kwangwoon University, Wolgye, Nowon, Seoul 139-701 (Korea, Republic of); Labuda, J. [Institute of Analytical Chemistry, Slovak University of Technology in Bratislava, 81237 Bratislava (Slovakia); Sillanpaeae, M. [University of Eastern Finland, Laboratory of Applied Environmental Chemistry (LAEC), Patteristonkatu 1, FI-50100 Mikkeli (Finland); LUT Faculty of Technology, Lappeenranta University of Technology, Patteristonkatu 1, FI-50100 Mikkeli (Finland)

    2010-12-15

    Novel CdS hollow microspheres have been successfully synthesized via a facile template-free solution-phase reaction from cadmium nitrate and thioacetamide precursors. The morphology of CdS hollow microspheres depends strongly on the ratio between the precursors, cadmium nitrate to thioacetamide ratio. The physical properties of the hollow microspheres have systematically been studied by different characterization methods. The stoichiometry of the hollow microspheres studied by the energy dispersive X-ray diffraction spectroscopy confirmed that the synthesized CdS hollow microspheres are nearly stoichiometric bulk like CdS. The morphology of the hollow microspheres studied by high resolution scanning electron microscopy and transmission electron microscopy observations showed that the CdS hollow microspheres of the size of 2.5 {mu}m have hollow structure and are constructed by several nanoparticles of the size between 30 and 40 nm. The UV-visible diffuse reflectance spectroscopy studies showed that the band gap of the CdS hollow microspheres increased while increasing the cadmium nitrate to thioacetamide ratio. Further electrochemical characterization of CdS hollow microspheres was performed with glassy carbon electrode (GCE) after its chemical modification by CdS dispersed in dimethylformamide. The electrochemical studies showed that with decreasing the band gap energy the electron transfer resistance of CdS/GCE was also found decreased. Moreover, electrochemical impedance spectroscopic measurements showed enhanced DNA adsorption onto CdS/GCE in comparison to GCE. These experiments demonstrate that the CdS hollow microspheres act as an efficient electrode modifier that effectively decreased the charge transfer resistance and capacitance of the modified sensors, which can be used for electroanalytical purposes.

  5. Fluoride adsorption studies on mixed-phase nano iron oxides prepared by surfactant mediation-precipitation technique.

    Science.gov (United States)

    Mohapatra, M; Rout, K; Singh, P; Anand, S; Layek, S; Verma, H C; Mishra, B K

    2011-02-28

    Mixed nano iron oxides powder containing goethite (α-FeOOH), hematite (α-Fe(2)O(3)) and ferrihydrite (Fe(5)HO(8)·4H(2)O) was synthesized through surfactant mediation-precipitation route using cetyltrimethyl ammonium bromide (CTAB). The X-ray diffraction, FTIR, TEM, Mössbauer spectroscopy were employed to characterize the sample. These studies confirmed the nano powder contained 77% goethite, 9% hematite and 14% ferrihydrite. Fluoride adsorption onto the synthesized sample was investigated using batch adsorption method. The experimental parameters chosen for adsorption studies were: pH (3.0-10.0), temperature (35-55°C), concentrations of adsorbent (0.5-3.0 g/L), adsorbate (10-100 mg/L) and some anions. Adsorption of fluoride onto mixed iron oxide was initially very fast followed by a slow adsorption phase. By varying the initial pH in the range of 3.0-10.0, maximum adsorption was observed at a pH of 5.75. Presence of either SO(4)(2-) or Cl(-) adversely affected the adsorption of fluoride in the order of SO(4)(2-)>Cl(-). The FTIR studies of fluoride loaded adsorbent showed that partly the adsorption on the surface took place at surface hydroxyl sites. Mössbauer studies indicated that the overall absorption had gone down after fluoride adsorption that implies it has reduced the crystalline bond strength. The relative absorption area of ferrihydrite was marginally increased from 14 to 17%. Copyright © 2010 Elsevier B.V. All rights reserved.

  6. Phase stability and grain growth in an Ag/Bi-2223 composite conductor prepared using fine-grained Bi-2223 as a precursor.

    Energy Technology Data Exchange (ETDEWEB)

    Merchant, N. N.

    1998-09-17

    We have investigated the stability and microstructural transformability of the Bi-2223 phase in a silver-sheathed monofilament composite tape fabricated using fine-grained Bi{sub 1.7}Pb{sub 0.3}Sr{sub 1.9}Ca{sub 2.0}-Cu{sub 3.0}O{sub y} (Bi-2223) as the precursor powder. The fully formed Bi-2223 precursor was prepared using established procedures. The purpose of this study was to explore the prospects for growing textured, large-grain-size Bi-2223 from the fine-grained precursor by process parameter perturbations. These perturbations included thermal ramp up variations, programmed heat treatment temperature and oxygen pressure fluctuations, and parameter manipulations during cool-down. Our results show that the types of heat treatments used in conventional oxide-powder-in-tube (OPIT) processing do not facilitate Bi-2223 grain growth when the precursor powder is preconcerted Bi-2223. We also observed that the Bi-2223 partially. decomposed during conventional thermal ramp-up in 0.075 atm O{sub 2}, but that this decomposition can be inhibited by ramping up in a reduced oxygen pressure. A pathway was found for back-reacting the fine-grained Bi-2223 (to Bi-2212, Bi-2201 and nonsuperconducting secondary phases), then reforming large-grained Bi-2223 in a colony microstructure having some distinct differences from that produced during conventional OPIT processing.

  7. Preparation of a pipette tip-based molecularly imprinted solid-phase microextraction monolith by epitope approach and its application for determination of enkephalins in human cerebrospinal fluid.

    Science.gov (United States)

    Li, Hua; Li, Dan

    2015-11-10

    In this study, a novel molecularly imprinted polymer (MIP) monolith for highly selective extraction of enkephalins was synthesized and prepared in a micropipette tip using epitope imprinting technique. The synthesized MIPs were characterized by scanning electron microscope (SEM) and infrared spectroscopy. A molecularly imprinted solid-phase microextraction (MISPME) method was developed for extraction of enkephalins in aqueous solutions. The parameters affecting MISPME were optimized. The results indicated that this MIP monolith exhibited specific recognition capability, high enrichment efficiency and excellent reusability for enkephalins. MALDI-TOF MS analysis demonstrated that this MIP monolith can act as a useful tool for highly selective purification and enrichment of enkephalin, a kind of low abundance protein, from high-abundance proteins in human cerebrospinal fluids (CSF). Employed this MIP monolith as solid-phase microextraction column, quantitative assay of enkephalins in human CSF was developed by HPLC-ultraviolet (UV) detection in this work. The detection limits were 0.05-0.08nM. This MISPME/HPLC-UV method was used to quantify Met-enkephalin and Leu-enkephalin levels in the CSF of patients with cancer pain.

  8. Preparation and characterization of magnetic carboxylated nanodiamonds for vortex-assisted magnetic solid-phase extraction of ziram in food and water samples.

    Science.gov (United States)

    Yılmaz, Erkan; Soylak, Mustafa

    2016-09-01

    A simple and rapid vortex-assisted magnetic solid phase extraction (VA-MSPE) method for the separation and preconcentration of ziram (zinc dimethyldithiocarbamate), subsequent detection of the zinc in complex structure of ziram by flame atomic absorption spectrometry (AAS) has been developed. The ziram content was calculated by using stoichiometric relationship between the zinc and ziram. Magnetic carboxylated nanodiamonds (MCNDs) as solid-phase extraction adsorbent was prepared and characterized by Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD) spectrometry and scanning electron microscopy (SEM). These magnetic carboxylated nanodiamonds carrying the ziram could be easily separated from the aqueous solution by applying an external magnetic field; no filtration or centrifugation was necessary. Some important factors influencing the extraction efficiency of ziram such as pH of sample solution, amount of adsorbent, type and volume of eluent, extraction and desorption time and sample volume were studied and optimized. The total extraction and detection time was lower than 10min The preconcentration factor (PF), the precision (RSD, n=7), the limit of detection (LOD) and limit of quantification (LOQ) were 160, 7.0%, 5.3µgL(-1) and 17.5µgL(-1), respectively. The interference of various ions has been examined and the method has been applied for the determination of ziram in various waters, foodstuffs samples and synthetic mixtures.

  9. Preparation and evaluation of a molecularly imprinted sol-gel material as the solid-phase extraction adsorbents for the specific recognition of cloxacilloic acid in cloxacillin.

    Science.gov (United States)

    Du, Kangli; Luo, Zhimin; Guo, Pengqi; Tang, Weili; Wu, Ningli; Zheng, Penglei; Du, Wei; Zeng, Aiguo; Jing, Wanghui; Chang, Chun; Fu, Qiang

    2016-02-01

    Highly selective molecularly imprinted polymers on the surface of silica gels were prepared by a sol-gel process and used as solid-phase extraction adsorbents for the specific recognition, enrichment and detection of cloxacilloic acid in cloxacillin. The obtained polymers were characterized by scanning electron microscopy, FTIR spectroscopy, nitrogen adsorption and desorption, elemental analysis and thermogravimetric analysis. The imprinted polymers not only possessed high adsorption capacity (6.5 μg/mg), but also exhibited fast adsorption kinetics (they adsorb 80% of the maximum amount within 20 min) and excellent selectivity (the imprinted factor was 3.6). A method using the imprinted polymers as solid-phase extraction adsorbents coupled with high-performance liquid chromatography was established with good specificity, linearity (r = 0.9962), precision (ranging from 0.5 to 6.7%), accuracy (ranging from 93.9 to 97.7%) and extraction recoveries (ranging from 78.8 to 89.8%). The limits of detection and quantification were 0.07 and 0.25 mg/g, respectively. This work could provide a promising method in the enrichment, extraction and detection of allergenic impurities in the manufacture, storage and application of cloxacillin.

  10. Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample.

    Science.gov (United States)

    He, Juan; Lv, Ruihe; Zhan, Haijun; Wang, Huizhi; Cheng, Jie; Lu, Kui; Wang, Fengcheng

    2010-07-26

    A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L(-1). The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

  11. Preparation of magnetic chitosan and graphene oxide-functional guanidinium ionic liquid composite for the solid-phase extraction of protein

    Energy Technology Data Exchange (ETDEWEB)

    Ding, Xueqin; Wang, Yuzhi, E-mail: wyzss@hnu.edu.cn; Wang, Ying; Pan, Qi; Chen, Jing; Huang, Yanhua; Xu, Kaijia

    2015-02-25

    Highlights: • A strategy for the solid-phase extraction of protein based on magnetic chitosan and graphene oxide-functional guanidinium ionic liquids. • Trypsin, lysozyme, ovalbumin and bovine serum albumin were used as the analyst. • The possibility of reusability and regeneration has been evaluated. - Abstract: A series of novel cationic functional hexaalkylguanidinium ionic liquids and anionic functional tetraalkylguanidinium ionic liquids have been synthesized, and then magnetic chitosan graphene oxide (MCGO) composite has been prepared and coated with these functional guanidinium ionic liquids to extract protein by magnetic solid-phase extraction. MCGO-functional guanidinium ionic liquid has been characterized by vibrating sample magnetometer, field emission scanning electron microscopy, X-ray diffraction spectrometer and Fourier transform infrared spectrometer. After extraction, the concentrations of protein were determined by measuring the absorbance at 278 nm using an ultra violet visible spectrophotometer. The advantages of MCGO-functional guanidinium ionic liquid in protein extraction were compared with magnetic chitosan, graphene oxide, MCGO and MCGO-ordinary imidazolium ionic liquid. The proposed method has been applied to extract trypsin, lysozyme, ovalbumin and bovine serum albumin. A comprehensive study of the adsorption conditions such as the concentration of protein, the amount of MCGO-functional guanidinium ionic liquid, the pH, the temperature and the extraction time were also presented. Moreover, the MCGO-functional guanidinium ionic liquid can be easily regenerated, and the extraction capacity was about 94% of the initial one after being used three times.

  12. Preparation and characterizations of HDPE-EVA alloy/OMT nanocomposites/paraffin compounds as a shape stabilized phase change thermal energy storage material

    Energy Technology Data Exchange (ETDEWEB)

    Cai Yibing [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, 230027 Anhui (China); Hu Yuan [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, 230027 Anhui (China)]. E-mail: yuanhu@ustc.edu.cn; Song Lei [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, 230027 Anhui (China); Lu Hongdian [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, 230027 Anhui (China); Chen Zuyao [Department of Chemistry, University of Science and Technology of China, Hefei, 230026 Anhui (China); Fan Weicheng [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, 230027 Anhui (China)

    2006-12-01

    A kind of shape stabilized phase change nanocomposites materials (PCNM) based on high density polyethylene (HDPE)/ethylene-vinyl acetate (EVA) alloy, organophilic montmorillonite (OMT), paraffin and intumescent flame retardant (IFR) are prepared using twin-screw extruder technique. The structures of the HDPE-EVA alloy/OMT nanocomposites are evidenced by the X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that an ordered intercalated nanomorphology of the HDPE-EVA alloy/OMT nanocomposites is formed. Then the structures of the shape stabilized PCNM are characterized by scanning electron microscopy (SEM). The HDPE-EVA alloy/OMT nanocomposites act as the supporting material and form the three-dimensional network structure. The paraffin acts as a phase change material and disperses in the three-dimensional network structure. Its latent heat is given by differential scanning calorimeter (DSC) method. The SEM and DSC results show that the additives of IFR have little effect on the network structure and the latent heat of shape stabilized PCNM, respectively. The thermal stability properties are characterized by thermogravimetric analysis (TGA). The TGA analysis results indicate that the flame retardant shape stabilized PCNM produce a larger amount of char residue at 800 deg. C than that of shape stabilized PCNM, although the onset of weight loss of the flame retardant shape stabilized PCNM occur at a lower temperature. The formed multicellular char residue contributes to the improvement of thermal stability performance. The probable combustion mechanisms are also discussed in this paper.

  13. Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

    Energy Technology Data Exchange (ETDEWEB)

    He Juan, E-mail: juanhe@haut.edu.cn [School of Chemistry and Chemical Engineering, Henan University of, Technology, LianHua Road, Zhengzhou 450051 (China); Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng [School of Chemistry and Chemical Engineering, Henan University of, Technology, LianHua Road, Zhengzhou 450051 (China)

    2010-07-26

    A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L{sup -1}. The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

  14. Preparation, Mechanical and Thermal Properties of Cement Board with Expanded Perlite Based Composite Phase Change Material for Improving Buildings Thermal Behavior

    Directory of Open Access Journals (Sweden)

    Rongda Ye

    2015-11-01

    Full Text Available Here we demonstrate the mechanical properties, thermal conductivity, and thermal energy storage performance of construction elements made of cement and form-stable PCM-Rubitherm® RT 28 HC (RT28/expanded perlite (EP composite phase change materials (PCMs. The composite PCMs were prepared by adsorbing RT28 into the pores of EP, in which the mass fraction of RT28 should be limited to be no more than 40 wt %. The adsorbed RT28 is observed to be uniformly confined into the pores of EP. The phase change temperatures of the RT28/EP composite PCMs are very close to that of the pure RT28. The apparent density and compression strength of the composite cubes increase linearly with the mass fraction of RT28. Compared with the thermal conductivity of the boards composed of cement and EP, the thermal conductivities of the composite boards containing RT28 increase by 15%–35% with the mass fraction increasing of RT28. The cubic test rooms that consist of six boards were built to evaluate the thermal energy storage performance, it is found that the maximum temperature different between the outside surface of the top board with the indoor temperature using the composite boards is 13.3 °C higher than that of the boards containing no RT28. The thermal mass increase of the built environment due to the application of composite boards can contribute to improving the indoor thermal comfort and reducing the energy consumption in the buildings.

  15. Silk fibroin/sodium alginate composite nano-fibrous scaffold prepared through thermally induced phase-separation (TIPS) method for biomedical applications

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Haiping, E-mail: zhp9810_a@163.com; Liu, Xiaotian, E-mail: xtianliu@126.com; Yang, Mingying, E-mail: yangm@zju.edu.cn; Zhu, Liangjun, E-mail: ljzhu@zju.edu.cn

    2015-10-01

    To mimic the natural fibrous structure of the tissue extracellular matrix, a nano-fibrous silk fibroin (SF)/sodium alginate (SA) composite scaffold was fabricated by a thermally-induced phase-separation method. The effects of SF/SA ratio on the structure and the porosity of the composite scaffolds were examined. Scanning electron microscopy and porosity results showed that the 5SF/1SA and 3SF/1SA scaffolds possessed an excellent nano-fibrous structure and a porosity of more than 90%. Fourier transform infrared, X-ray diffraction, and differential scanning calorimetry results indicated the physical interaction between SF and SA molecules and their good compatibility in the 5SF/1SA and 3SF/1SA scaffolds, whereas they showed less compatibility in the 1SF/1SA scaffold. Cell culture results showed that MG-63 cells can attach and grow well on the surface of the SF/SA scaffolds. The nano-fibrous SF/SA scaffold can be potentially used in tissue engineering. - Highlights: • We fabricate a nano-fibrous silk fibroin (SF)/sodium alginate (SA) composite scaffold. • The scaffold was prepared through a thermally induced phase separation method. • SF molecules are physically interacted with SA molecules. • Good molecular compatibility can be found in 5SF/1SA and 3SF/1SA scaffolds. • The nano-fibrous SF/SA scaffold is biocompatible.

  16. Butanol Dehydration over V2O5-TiO2/MCM-41 Catalysts Prepared via Liquid Phase Atomic Layer Deposition

    Directory of Open Access Journals (Sweden)

    Jong-Ki Jeon

    2013-04-01

    Full Text Available MCM-41 was used as a support and, by using atomic layer deposition (ALD in the liquid phase, a catalyst was prepared by consecutively loading titanium oxide and vanadium oxide to the support. This research analyzes the effect of the loading amount of vanadium oxide on the acidic characteristics and catalytic performance in the dehydration of butanol. The physical and chemical characteristics of the TiO2-V2O5/MCM-41 catalysts were analyzed using XRF, BET, NH3-TPD, XRD, Py-IR, and XPS. The dehydration reaction of butanol was performed in a fixed bed reactor. For the samples with vanadium oxide loaded to TiO2/MCM-41 sample using the liquid phase ALD method, it was possible to increase the loading amount until the amount of vanadium oxide reached 12.1 wt %. It was confirmed that the structural properties of the mesoporous silica were retained well after titanium oxide and vanadium loading. The NH3-TPD and Py-IR results indicated that weak acid sites were produced over the TiO2/MCM-41 samples, which is attributed to the generation of Lewis acid sites. The highest activity of the V2O5(12.1-TiO2/MCM-41 catalyst in 2-butanol dehydration is ascribed to it having the highest number of Lewis acid sites, as well as the highest vanadium dispersion.

  17. Study and development of reversed-phase HPLC systems for the determination of 2-imidazolines in the presence of preservatives in pharmaceutical preparations.

    Science.gov (United States)

    Antoniou, Constantinos G; Markopoulou, Catherine K; Kouskoura, Maria G; Koundourellis, John E

    2011-01-01

    Different HPLC chromatographic systems were investigated on a C18 ACE 5 pm, 150 x 4.6 mm id column for the determination of tymazoline, tramazoline, and antazoline, with either naphazoline or xylometazoline, in commercial preparations. For the development and optimization of the systems, a Response Surface Method (r=0.925-0.980) was used to illustrate the changes in k as a function of pH values and different salt concentrations. The simultaneous separation of 2-imidazolines was accomplished at 40 degrees C with 0.01 M ammonium acetate-methanol (50+50, v/v, pH 6.0) mobile phase at a flow rate of 1.2 mL/min. In order to deal with the usual coexistence of 2-imidazolines with benzethonium and benzalkonium chloride preservatives, it was necessary to use another chromatographic system, 0.01 M ammonium acetate-methanol (50+50, v/v) mobile phase on a cyano ACE 5 pm, 150 x 4.6 mm id column. As part of a more thorough theoretical investigation, a partial least-squares (PLS) technique was used for modeling the RP-HPLC retention data. The model was based on molecular structure descriptors of the analytes' X variables and on their retention time (Log K) Y. The goodness of fit was estimated by the PLS correlation coefficient (r2) and root mean square error of estimation values, which were 0.994 and 0.0479, respectively.

  18. The timing of the human circadian clock is accurately represented by the core body temperature rhythm following phase shifts to a three-cycle light stimulus near the critical zone

    Science.gov (United States)

    Jewett, M. E.; Duffy, J. F.; Czeisler, C. A.

    2000-01-01

    A double-stimulus experiment was conducted to evaluate the phase of the underlying circadian clock following light-induced phase shifts of the human circadian system. Circadian phase was assayed by constant routine from the rhythm in core body temperature before and after a three-cycle bright-light stimulus applied near the estimated minimum of the core body temperature rhythm. An identical, consecutive three-cycle light stimulus was then applied, and phase was reassessed. Phase shifts to these consecutive stimuli were no different from those obtained in a previous study following light stimuli applied under steady-state conditions over a range of circadian phases similar to those at which the consecutive stimuli were applied. These data suggest that circadian phase shifts of the core body temperature rhythm in response to a three-cycle stimulus occur within 24 h following the end of the 3-day light stimulus and that this poststimulus temperature rhythm accurately reflects the timing of the underlying circadian clock.

  19. 织物整理用相变微胶囊的制备%Preparation of phase change micro-capsules for textile finishing

    Institute of Scientific and Technical Information of China (English)

    闫飞; 陆大年

    2011-01-01

    为了使微胶囊的粒径分布变窄、减小体均粒径,提高其储热性能,更好地用于织物整理,在原有工作的基础上,利用超声波技术制备相变微胶囊,并研究超声波对相变微胶囊性能的影晌.结果表明:经超声波制备的微胶囊数均粒径为1.4μm,分布指数PDI为2.93,可以有效降低所制备相变微胶囊的体均粒径和分散程度,利用该相变微胶囊整理的织物具有较好的智能调温作用.%In order to narrow the size distribution of micro-capsules, shorten the body average particle size,increase the heat storage property and make it better for the textiie finishing, phase change micro-capsules (MCPCMs) were prepared with ultrasonic technology based on the original work.The effect of ultrasonic on the properlies of phase change micro-capsules was investigated.The results showed that the number average particle size of micro-capsules was about 1.4 μm, distribution index PDI was 2.93.The body average particle size of phase change micro-capsules and dispersion degree could be effectively decreased.The MCPCMs finished fabric showed good intellectual temperature-control function.

  20. [Selection of mobile phases for the determination of gamma-schisandrin and multi-active constituents in Schisandra chinensis and its preparations by high performance liquid chromatography].

    Science.gov (United States)

    Yang, Xiaorong; Xiang, Qingxiang; Chen, Jiaxuan

    2009-05-01

    The systems of mobile phase for the determination of gamma-schisandrin in Schisandra chinensis and its preparations were developed by high performance liquid chromatography (HPLC). The separation was performed on a Shim-pack VP-ODS column (250 mm x 4.6 mm, 5 microm) at 30 degrees C, the detection wavelength was set at 285 nm and the flow rate was 1.0 mL/min. Retention times and separation were investigated in mixed solution of three reference substances (gamma-schisandrin, anwulignan, and deoxyschizandrin) and methanol extract of Schisandra chinensis by different systems and proportions of mobile phases to select optimal conditions for the determination of gamma-schisandrin. The results showed that the complete separation of gamma-schisandrin and anwulignan was difficult in the systems of methanol-water and methanol-acetic acid-water. The separation of gamma-schisandrin, anwulignan and deoxyschizandrin can be completed in the systems of acetonitrile-methanol-water and acetonitrile-acetic acid-water when their proportions were suitable. The mobile phase of acetonitrile-methanol-water (17:58:25, v/v/v) was selected for the determination of deoxyschizandrin, gamma-schisandrin and anwulignan in Schisandra chinensis and Hugan tablets. The determination results of the three substances were satisfactory with the relative standard deviations (n = 4) ranged from 0.95% to 5.8%, and the average recoveries ranged from 94.50% to 105.6%. The efficiency of separation and the results of determination were satisfactory for the real samples.

  1. Preparation and Supercooling Modification of Salt Hydrate Phase Change Materials Based on CaCl₂·2H₂O/CaCl₂.

    Science.gov (United States)

    Xu, Xiaoxiao; Dong, Zhijun; Memon, Shazim Ali; Bao, Xiaohua; Cui, Hongzhi

    2017-06-23

    Salt hydrates have issues of supercooling when they are utilized as phase change materials (PCMs). In this research, a new method was adopted to prepare a salt hydrate PCM (based on a mixture of calcium chloride dihydrate and calcium chloride anhydrous) as a novel PCM system to reduce the supercooling phenomenon existing in CaCl₂·6H₂O. Six samples with different compositions of CaCl₂ were prepared. The relationship between the performance and the proportion of calcium chloride dihydrate (CaCl₂·2H₂O) and calcium chloride anhydrous (CaCl₂) was also investigated. The supercooling degree of the final PCM reduced with the increase in volume of CaCl₂·2H₂O during its preparation. The PCM obtained with 66.21 wt % CaCl₂·2H₂O reduced the supercooling degree by about 96.8%. All six samples, whose ratio of CaCl₂·2H₂O to (CaCl₂ plus CaCl₂·2H₂O) was 0%, 34.03%, 53.82%, 76.56%, 90.74%, and 100% respectively, showed relatively higher enthalpy (greater than 155.29 J/g), and have the possibility to be applied in buildings for thermal energy storage purposes. Hence, CaCl₂·2H₂O plays an important role in reducing supercooling and it can be helpful in adjusting the solidification enthalpy. Thereafter, the influence of adding different percentages of Nano-SiO₂ (0.1 wt %, 0.3 wt %, 0.5 wt %) in reducing the supercooling degree of some PCM samples was investigated. The test results showed that the supercooling of the salt hydrate PCM in Samples 6 and 5 reduced to 0.2 °C and 0.4 °C respectively. Finally, the effect of the different cooling conditions, including frozen storage (-20 °C) and cold storage (5 °C), that were used to prepare the salt hydrate PCM was considered. It was found that both cooling conditions are effective in reducing the supercooling degree of the salt hydrate PCM. With the synergistic action of the two materials, the performance and properties of the newly developed PCM systems were better especially in terms of reducing

  2. Representing distance, consuming distance

    DEFF Research Database (Denmark)

    Larsen, Gunvor Riber

    to mobility and its social context. Such an understanding can be approached through representations, as distance is being represented in various ways, most noticeably in maps and through the notions of space and Otherness. The question this talk subsequently asks is whether these representations of distance...... are being consumed in the contemporary society, in the same way as places, media, cultures and status are being consumed (Urry 1995, Featherstone 2007). An exploration of distance and its representations through contemporary consumption theory could expose what role distance plays in forming...... are present in theoretical and empirical elaborations on mobility, but these remain largely implicit and unchallenged (Bauman 1998). This talk will endeavour to unmask distance as a theoretical entity by exploring ways in which distance can be understood and by discussing distance through its representations...

  3. Application of colloidal chemistry in aqueous phase to the preparation of supported metallic catalysts: particles size and aggregation control; Application de la chimie colloidale en phase aqueuse a la preparation de catalyseurs metalliques supportes: controle de la taille et de l`etat d`agregation des particules

    Energy Technology Data Exchange (ETDEWEB)

    Pages, T.

    1998-09-16

    This work is an application of colloidal chemistry in aqueous phase on supported metal catalyst preparation. The objective is the control of particle size and aggregation. The preparation of the materials was achieved in two steps: - the synthesis of PdO hydrosols was obtained by two ways: neutralisation of the solution containing metallic salt by adding alkaline solution or by thermo-hydrolysis; the sols were then deposited on carriers (Al{sub 2}O{sub 3}, SIO{sub 2}). The use of partial charge model allowed us to determine the complexes that were able to generate PdO. The preparation of PdO from Pd(H{sub 2}O){sub 4}{sup 2+} was studied and a mechanism of oxide formation was elaborated. The neutralisation of Pd(H{sub 2}O){sub 4}{sup 2+} obtained by adding alkaline solution led to particles with an average size of 1.8 nm and a narrow particle size distribution. Only the thermo-hydrolysis of Pd(H{sub 2}O){sub 4}{sup 2+} led to particles which size is higher than 3.0 nm. In the last case, particle size is controlled by the precursor concentration (Pd(H{sub 2}O){sub 2}(OH){sub 2}) generated in the medium. We have demonstrated that particle aggregation in the sol depends on the Ph and the way of preparation. It can be controlled by adding complexing anions (Cl{sup -}, NO{sub 2}{sup -}). Concerning the deposition of sols on carriers, it led to isolated or aggregated particles according to experimental conditions. Particle size was not modified during the deposition. Moreover, in our experimental conditions, reduction of particles did not modify particle size and aggregation. An application of this original way of preparation on catalysis allowed us to demonstrate the interest of controlling particle size and aggregation. (author) 186 refs.

  4. Preparation of low flow-resistant methacrylate-based monolithic stationary phases of different hydrophobicity and the application to rapid reversed-phase liquid chromatographic separation of alkylbenzenes at high flow rate and elevated temperature.

    Science.gov (United States)

    Ueki, Yuji; Umemura, Tomonari; Iwashita, Yoshikazu; Odake, Tamao; Haraguchi, Hiroki; Tsunoda, Kin-ichi

    2006-02-17

    Low flow-resistant alkyl methacrylate-based monolithic stationary phases of different hydrophobicity were constructed for reversed-phase capillary liquid chromatography by thermally initiated radical polymerization of respective methacrylate ester monomer with different alkyl chain (C2, C4, C6, C12, C18) and ethylene glycol dimethacrylate (EDMA) in a 250 microm i.d. fused silica capillary. The hydrophobicity was basically controlled by changing the length and/or the density of the alkyl-chain, while the composition and the ratio of porogenic solvent were adjusted to obtain highly permeable rigid monoliths with adequate column efficiency. Among the prepared monolithic stationary phases, C18-methacrylate monoliths polymerized from a binary porogenic solvent of isoamyl alcohol and 1,4-buthandiol exhibited the most promising performance in terms of hydraulic resistance and column efficiency. The pressure drops of 20-cm long monolithic columns were below approximately 0.4 MPa at a normal linear velocity of 1mm/s (a flow rate of 3 microL/min), and the numbers of theoretical plates for alkylbenzenes mostly exceeded 3000 plates/20 cm. The produced monolithic columns had good mechanical strength for high pressure and temperature, and could be properly operated even at a temperature of 80 degrees C and at a pressure of at least 33 MPa. At 80 degrees C, the theoretical plate numbers reached 6000 plates/20 cm because of the enhanced mass transfer. Due to the novel hydraulic resistance and mechanical strength, the separation time could be reduced 120-fold simply by raising the flow rate and column temperature.

  5. Representativity of TMA studies.

    Science.gov (United States)

    Sauter, Guido

    2010-01-01

    The smaller the portion of a tumor sample that is analyzed becomes, the higher is the risk of missing important histological or molecular features that might be present only in a subset of tumor cells. Many researchers have, therefore, suggested using larger tissue cores or multiple cores from the same donor tissue to enhance the representativity of TMA studies. However, numerous studies comparing the results of TMA studies with the findings from conventional large sections have shown that all well-established associations between molecular markers and tumor phenotype or patient prognosis can be reproduced with TMAs even if only one single 0.6 mm tissue spot is analyzed. Moreover, the TMA technology has proven to be superior to large section analysis in finding new clinically relevant associations. The high number of samples that are typically included in TMA studies, and the unprecedented degree of standardization during TMA experiments and analysis often give TMA studies an edge over traditional large-section studies.

  6. Preparation of Solid Phase Microextraction (SPME) Probes through Polyaniline Multiwalled Carbon Nanotubes (PANI/MWCNTs) Coating for the Extraction of Palmitic Acid and Oleic Acid in Organic Solvents.

    Science.gov (United States)

    Khajeamiri, Alireza

    2012-01-01

    A fiber coating from polyaniline (PANI) was electrochemically prepared and employed for Solid phase micreoextraction (SPME). The PANI film was directly electrodeposited on the platinum wire surface using cyclic voltametry (CV) technique. The same method was applied for the preparation of SPME fiber coated by polyaniline multiwalled carbon nanotubes (PANI/MWCNTs) composite. The concentration of sulfuric acid for electropolymerization was 0.1 M in the presence of 0.045 M aniline in aqueous solution. For the electrodeposition of PANI/MWCNT composite, 4 μg/mL of MWCNTs was dispersed into the solution. Film coating was carried out on the platinum wire by repetitive cycling of potentials between 0 and 1.0 V at the scan rate of 0.05 V/s. The applicability of these coatings were assessed through employing a laboratory-made SPME injecting device and gas chromatography with mass spectrometry (GC-MS) for the extraction of palmitic acid and oleic acid from chloroform. The developed method proved to be simple and easy, offering high reproducibility. Both PANI coated and PANI/CNT coated probes had the ability to concentrate palmitic acid and oleic acid on their coating and produced strong signals in GC-MS chromatograms. In the meantime, PANI/CNT coated SPME probes produced signals which were stronger than those produced by PANI coated SPME probes. The amount of extracted palmitic acid and oleic acid from chloroform by the PANI/MWCNTs coating was about 6 and 12 times higher than the amount extracted by plane PANI SPME fibers respectively. It could be suggested that the composite material with CNTs has both an increased surface area and an elevated absorptive capacity which leads to this overall increase in extracted palmitic acid and oleic acid.

  7. Preparation of polypyrrole composite solid-phase microextraction fiber coatings by sol-gel technique for the trace analysis of polar biological volatile organic compounds.

    Science.gov (United States)

    Zhang, Zhuomin; Zhu, Li; Ma, Yunjian; Huang, Yichun; Li, Gongke

    2013-02-21

    Two novel polypyrrole (PPy) composite solid-phase microextraction (SPME) fiber coatings involving polypyrrole β-naphthalenesulfonic acid (PPy/β-NSA) and polypyrrole graphene (PPy/GR) composite SPME fiber coatings were prepared by a simple sol-gel technique for selectively sampling relatively polar biological volatile organic compounds (VOCs). Crucial preparation conditions of the PPy composite SPME fiber coatings were optimized and are discussed in detail. Physical tests suggested that the PPy composite SPME fiber coatings possessed a porous surface morphology, stable chemical and thermal properties. Due to the inducing polar functional groups in the PPy molecule, the PPy composite SPME fiber coatings achieved a higher extraction capacity and special selectivity for the polar biological VOCs with conjugate structures, compared with commercial SPME fiber coatings. Enrichment factors of most of the VOCs by the PPy/β-NSA and PPy/GR SPME fibers were much higher than those achieved by common commercially available SPME fiber coatings. Finally, the PPy/β-NSA and PPy/GR SPME fiber coatings were applied for the trace analysis of typical polar VOCs from ant and coriander samples coupled with gas chromatography/mass spectrometry (GC/MS) detection, respectively. It was satisfactory that the average contents of 4-heptanone, 4-heptanol, 4-nonanone and methyl 5-methylsalicylate from ant samples were actually found to be 28.0, 58.7, 3.0 and 0.6 μg g(-1), and the average contents of nonane, decanal, undecanal and dodecanal from coriander samples were actually found to be 0.79, 0.13, 0.06 and 0.21 μg g(-1). The results suggested that PPy composite SPME coatings will be a potentially excellent sampling technique for the trace analysis of polar biological VOCs.

  8. Effects of post-deposition heat treatment on the microstructure and properties of Al-doped ZnO thin films prepared by aqueous phase deposition

    Energy Technology Data Exchange (ETDEWEB)

    Yao, Pin-Chuan, E-mail: pcyao@mail.dyu.edu.tw [Department of Materials Science and Engineering, Da-Yeh University, Dacun, Changhua 51591, Taiwan (China); Hang, Shih-Tse; Wu, Menq-Jiun [Department of Mechatronics Engineering, National Changhua University of Education, Changhua 50007, Taiwan (China); Hsiao, Wen-Tse [Instrument Technology Research Center, National Applied Research Laboratories, Hsinchu 30076, Taiwan (China)

    2012-01-31

    In this study, transparent conducting aluminum-doped ZnO thin films (AZO) were deposited on glass substrates by a water-based liquid phase deposition method. The results show that by employing a two-step post-deposition heat treatment, the preferential orientation of ZnO (002) appeared as soon as the polycrystalline films were formed. Under a reducing atmosphere, the crystallinity of the films was effectively improved. Furthermore, the reducing atmosphere was also beneficial for the removal of the residual stress of the prepared films and the c-axis lattice constant was less stretched as compared to those under an inert atmosphere at identical T{sub p}. Both the atomic force micrograph and scanning electron micrograph clearly exhibited that the heat treatment induced considerable grain growth. The X-ray photoelectron spectrum revealed that the heat treatment atmosphere had little impact on the bonding state of zinc and that the reducing atmosphere was favorable for the non-stoichiometric alumina, which in turn, resulted in more oxygen vacancies and led to improvement in electrical conductivity. The ratio of chemisorbed oxygen declined substantially when applying the reducing atmosphere. Accordingly, hydrogen was helpful for the reduction of chemisorbed oxygen onto AZO films. Generally, the electrical resistivity declined linearly with T{sub p}. A minimum resistivity of 9.90 Multiplication-Sign 10{sup -3} {Omega}{center_dot}cm was obtained with a doping concentration of Al/Zn = 2.25 at.% at T{sub p} = 700 Degree-Sign C. The largest mean free path of the carriers was 1.2 A, which was much smaller than the observed grain sizes of the AZO films. Accordingly, the grain boundary scattering was not the detrimental scattering mechanism. In contrast, the scattering within the grains was responsible for the low mobility. An increase in optical transparency with the heat treatment temperature was observed due to the compact and smooth topography with larger grains, among

  9. Preparation of manganese oxide immobilized on SBA-15 by atomic layer deposition as an efficient and reusable catalyst for selective oxidation of benzyl alcohol in the liquid phase

    Energy Technology Data Exchange (ETDEWEB)

    Mahdavi, Vahid, E-mail: v-mahdavi@araku.ac.ir; Mardani, Mahdieh

    2015-04-01

    Manganese oxide supported on mesoporous silica SBA-15 catalyst (Mn-SBA-15) was tested with Mn contents in the range of 0.8–23 wt%. Samples were prepared by the controlled grafting process of atomic layer deposition (ALD). Other sample was prepared for comparisons by the wet impregnation method. These samples were characterized by the techniques of ICP, XRD, SEM, Raman, FT-IR spectroscopy, diffuse reflectance UV–Vis, TGA-DSC, and N{sub 2} absorption–desorption surface area measurement. Results indicated that anchored manganese oxide particles have been successfully synthesized over the surface of SBA-15. These samples contained Red-Ox ion pairs of Mn{sup 2+} and Mn{sup 3+} highly dispersed on the mesoporous silica surface. The impregnated sample exhibited lower surface area and contained Red-Ox ion pairs of Mn{sup 3+} and Mn{sup 4+} more aggregated particles on the SBA-15 surface. Results determined Mn-SBA-15 as an efficient and selective catalyst for oxidation of benzyl alcohol with tert-butylhydroperoxide in liquid phase. In accordance with expectations, there was a negligible amount of leaching of immobilized manganese oxide from the support during the reaction, because of strong surface interaction between manganese oxide and hydroxyls groups. The influences of reaction temperature, reaction time, solvent, TBHP/benzyl alcohol molar ratio, amount of catalyst and reusability were investigated. Under optimized conditions (0.2 g catalyst, TBHP/benzyl alcohol molar ratio 1, solvent acetonitrile; T = 90 °C; reaction time 8 h), results achieved 70% conversion of benzyl alcohol and 100% selectivity to benzaldehyde. - Highlights: • Manganese oxide immobilized on SBA-15 were prepared by atomic layer deposition (ALD). • Oxidation of benzyl alcohol to benzaldehyde over this catalyst were investigated. • Effects of loading of manganese oxide, T, oxidant/alcohol ratio were investigated. • The leaching of manganese oxide from support during the reaction was

  10. Enhanced thermionic emission properties in textured two-phase LaB{sub 6}–BaB{sub 6} system prepared by spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Shen Lin, E-mail: shenlinz@sina.com [College of Mathematics and Physics, Jinggangshan University, Jian 343409 (China); Shanghai Key Laboratory of Special Artificial Microstructure and Pohl Institute of Solid State Physics and School of Physics Science and Engineering, Tongji University, Shanghai 200092 (China); State Key Laboratory of Theoretical Physics, Institute of Theoretical Physics, Chinese Academy of Sciences, Beijing 100190 (China); Zhang, Jiu Xing, E-mail: zjiuxing@hfut.edu.cn [School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009 (China); Bao, Li Hong [Inner Mongolia Key Laboratory for Physics and Chemistry of Functional Materials, Inner Mongolia Normal University, Hohhot 010022 (China); Yu, Xiao Guang; Hu, Qiang Lin; Hu, Dong Qiang [College of Mathematics and Physics, Jinggangshan University, Jian 343409 (China)

    2014-10-25

    Graphical abstract: Room temperature XRD patterns of the nominal composition (La{sub 0.6}Ba{sub 0.4})B{sub 6} synthesized by SPS at 1400 °C for 5 min under 50 MPa. The XRD patterns reveal that the (La{sub 0.6}Ba{sub 0.4})B{sub 6} is a two-phase mixture of LaB{sub 6} and BaB{sub 6}. The inset is a macroscopic picture of the obtained (La{sub 0.6}Ba{sub 0.4})B{sub 6}. - Highlights: • (La{sub 0.6}Ba{sub 0.4})B{sub 6} has been successfully prepared by spark plasma sintering. • The obtained (La{sub 0.6}Ba{sub 0.4})B{sub 6} compound is a two-phase mixture of LaB{sub 6} and BaB{sub 6}. • The (0 0 1) texture is favorable for the decrease of work function. • The addition of BaB{sub 6} to LaB{sub 6} improves the electron emission performance. • (La{sub 0.6}Ba{sub 0.4})B{sub 6} is shown to be promising candidate for cathode applications. - Abstract: Structure, crystallographic orientation, and thermionic emission properties of the two-phase LaB{sub 6}–BaB{sub 6} system fabricated by a combined process of evaporation–condensation and spark plasma sintering (SPS) were investigated systematically. The powder X-ray diffraction (XRD) reveals that the obtained nominal composition (La{sub 0.6}Ba{sub 0.4})B{sub 6} compound exhibits coexistence of two isostructural phases of LaB{sub 6} and BaB{sub 6}. The electron backscatter diffraction (EBSD) confirms that the surface of the (La{sub 0.6}Ba{sub 0.4})B{sub 6} forms a clear (0 0 1) texture, which favors reduction in work function. Thermionic emission properties were measured in the temperature range between 1500 and 1873 K. The results indicated that the (La{sub 0.6}Ba{sub 0.4})B{sub 6} emitter displayed a low work function of 1.95 eV, and a high zero field emission current density of 10 A cm{sup −2} at 1773 K. Compared to the reported LaB{sub 6} and (La{sub 0.6}Sm{sub 0.4})B{sub 6} prepared for identical synthesis conditions, (La{sub 0.6}Ba{sub 0.4})B{sub 6} is shown to have the most excellent thermionic emission

  11. 采用特殊的相反转乳化剂制备水基环氧固化剂分散体%Preparation of aqueous dispersion of epoxy curing agent with specially synthesized phase inversion emulsifier

    Institute of Scientific and Technical Information of China (English)

    周继亮; 涂伟萍; 胡剑青

    2005-01-01

    Generally, the curing agents for aqueous ambient-temperature-cured epoxy resin systems are epoxy-polyamine adduct, which are rendered water-soluble by salting with organic acids,while these acids have adverse influence on film property.It is a trend to develop aqueous dispersion of epoxy curing agent free of organic acids.The conventional surfactants are not suited to act as phase inversion emulsifiers to prepare aqueous dispersion of epoxy-polyamine adduct. So a special phase inversion emulsifier TETA-DGEPG-EPON834 was synthesized in two steps.Firstly, diglycidyl ether of polyglycol(DGEPG) was used as the chain extender to react with triethylenete tramine(TETA) in propylene glycol methyl ether (PM) at 70℃ for about 4 h.Secondly, epoxy resin(EPON834) was used as the chain extender to react with the adduct of TETA-DGEPG in PM at 65℃ for about 3 h.Then the special phase inversion emulsifier was used to prepare aqueous dispersion of EPON828-TETA adduct terminated by E10. In circumstances of low emulsifier concentration (5%), phase inversion was not completed at phase inversion point (PIP) (0.35). While the phase inversion has completely finished at PIP (0.45) in the circumstances of high emulsifier concentration (10%).A stable aqueous dispersion of EPON828-TETA adduct terminated by E10 was prepared in circumstances of high emulsifier concentration (10%).

  12. Preparation and Phase Change Properties of Paraffin Microcapsules%石蜡相变微胶囊的制备及相变性能研究

    Institute of Scientific and Technical Information of China (English)

    李庆丹; 朱冬梅; 李娇娇; 罗发; 周万城

    2011-01-01

    以石蜡为芯材,蜜胺树脂(MF)为壁材,采用原位聚合法制备了石蜡相变微胶囊.分别采用傅立叶变换红外光谱仪(FTIR)、差示扫描苗热仪(DSC)和扫描电子显微镜(SEM)对微胶囊的结构、性能和形貌进行了分析和表征,讨论了甲醛与三聚氰胺的摩尔比对微胶囊相变性能和形貌的影响.结果表明,n(甲醛)/n(三聚氰胺)>4时,微胶囊之间发生粘结,出现了团聚现象;微胶囊的相变温度略高于芯材石蜡,随着n(甲醛)/n(三聚氰胺)增加,微胶囊的相变潜热降低.%The microcapsules containing paraffin were prepared through the in-sim polymerization method using melamine-formaldehyde as the wall material. The structures, properties and morphology of the microcapsules were characterized by fourier-transform infrared spectra (FTIR), differential scanning calorimeter (DSC) and scanning electronic microscope (SEM). The effects of the molar ratio of formaldehyde to melamine on the morphology and phase change properties of the microencapsulated paraffin were investigated. The results showed that when the molar ratio of formaldehyde to melamine was higher than 4, a high degree of cross-linking in the melamine-formaldehyde resin was obtained and the visible agglomeration of the microcapsules was observed. The phase-transforming point of microcapsules was higher than that of paraffin and the latent heat of microcapsules decreased as n (formaldehyde)/n (melamine) increased.

  13. Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples.

    Science.gov (United States)

    Bagheri, Habib; Aghakhani, Ali; Baghernejad, Masoud; Akbarinejad, Alireza

    2012-02-24

    A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100-200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2-10 ng L(-1). The relative standard deviations (RSD) (n=3) at the concentration level of 1.7-6.7 ng mL(-1) were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27-1330 ng L(-1) for phenol and monochlorophenols and 7-1000 ng L(-1) for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%. Copyright © 2011

  14. Preparation and characterizations of HDPE-EVA alloy/OMT nanocomposites/paraffin compounds as a shape stabilized phase change thermal energy storage material

    Energy Technology Data Exchange (ETDEWEB)

    Cai, Yibing; Hu, Yuan; Song, Lei; Lu, Hongdian; Fan, Weicheng [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, 230027 Anhui (China); Chen, Zuyao [Department of Chemistry, University of Science and Technology of China, Hefei, 230026 Anhui (China)

    2006-12-01

    A kind of shape stabilized phase change nanocomposites materials (PCNM) based on high density polyethylene (HDPE)/ethylene-vinyl acetate (EVA) alloy, organophilic montmorillonite (OMT), paraffin and intumescent flame retardant (IFR) are prepared using twin-screw extruder technique. The structures of the HDPE-EVA alloy/OMT nanocomposites are evidenced by the X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that an ordered intercalated nanomorphology of the HDPE-EVA alloy/OMT nanocomposites is formed. Then the structures of the shape stabilized PCNM are characterized by scanning electron microscopy (SEM). The HDPE-EVA alloy/OMT nanocomposites act as the supporting material and form the three-dimensional network structure. The paraffin acts as a phase change material and disperses in the three-dimensional network structure. Its latent heat is given by differential scanning calorimeter (DSC) method. The SEM and DSC results show that the additives of IFR have little effect on the network structure and the latent heat of shape stabilized PCNM, respectively. The thermal stability properties are characterized by thermogravimetric analysis (TGA). The TGA analysis results indicate that the flame retardant shape stabilized PCNM produce a larger amount of char residue at 800{sup o}C than that of shape stabilized PCNM, although the onset of weight loss of the flame retardant shape stabilized PCNM occur at a lower temperature. The formed multicellular char residue contributes to the improvement of thermal stability performance. The probable combustion mechanisms are also discussed in this paper. (author)

  15. Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Habib, E-mail: bagheri@sharif.edu [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of); Aghakhani, Ali; Baghernejad, Masoud; Akbarinejad, Alireza [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2012-02-24

    A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100-200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2-10 ng L{sup -1}. The relative standard deviations (RSD) (n = 3) at the concentration level of 1.7-6.7 ng mL{sup -1} were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27-1330 ng L{sup -1} for phenol and monochlorophenols and 7-1000 ng L{sup -1} for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%.

  16. Metastable tetragonal Cu2Se hyperbranched structures: large-scale preparation and tunable electrical and optical response regulated by phase conversion.

    Science.gov (United States)

    Zhu, Jinbao; Li, Qiuyang; Bai, Liangfei; Sun, Yongfu; Zhou, Min; Xie, Yi

    2012-10-08

    Despite the promising applications of copper selenide nanoparticles, an in-depth elucidation of the inherent properties of tetragonal Cu(2)Se (β-Cu(2)Se) has not been performed because of the lack of a facile synthesis on the nanoscale and an energy-intensive strategy is usually employed. In this work, a facile wet-chemical strategy, employing HCOOH as reducing agent, has been developed to access single-crystalline metastable β-Cu(2)Se hyperbranched architectures for the first time. The process avoids hazardous chemistry and high temperatures, and thus opens up a facile approach to the large-scale low-cost preparation of metastable β-Cu(2)Se hyperbranched architectures. A possible growth mechanism to explain the formation of the β-Cu(2)Se dendritic morphology has been proposed based on time-dependent shape evolution. Further investigations revealed that the metastable β-Cu(2)Se can convert into the thermodynamically more stable cubic α-Cu(2-x)Se maintaining the dendritic morphology. An increase in electrical conductivity and a tunable optical response were observed under ambient conditions. This behavior can be explained by the oxidation of the surface of the β-Cu(2)Se hyperbranched structures, ultimately leading to solid-state phase conversion from β-Cu(2)Se into superionic conductor α-Cu(1.8)Se, which has potential applications in energy-related devices and sensors.

  17. Preparation of magnetic chitosan and graphene oxide-functional guanidinium ionic liquid composite for the solid-phase extraction of protein.

    Science.gov (United States)

    Ding, Xueqin; Wang, Yuzhi; Wang, Ying; Pan, Qi; Chen, Jing; Huang, Yanhua; Xu, Kaijia

    2015-02-25

    A series of novel cationic functional hexaalkylguanidinium ionic liquids and anionic functional tetraalkylguanidinium ionic liquids have been synthesized, and then magnetic chitosan graphene oxide (MCGO) composite has been prepared and coated with these functional guanidinium ionic liquids to extract protein by magnetic solid-phase extraction. MCGO-functional guanidinium ionic liquid has been characterized by vibrating sample magnetometer, field emission scanning electron microscopy, X-ray diffraction spectrometer and Fourier transform infrared spectrometer. After extraction, the concentrations of protein were determined by measuring the absorbance at 278 nm using an ultra violet visible spectrophotometer. The advantages of MCGO-functional guanidinium ionic liquid in protein extraction were compared with magnetic chitosan, graphene oxide, MCGO and MCGO-ordinary imidazolium ionic liquid. The proposed method has been applied to extract trypsin, lysozyme, ovalbumin and bovine serum albumin. A comprehensive study of the adsorption conditions such as the concentration of protein, the amount of MCGO-functional guanidinium ionic liquid, the pH, the temperature and the extraction time were also presented. Moreover, the MCGO-functional guanidinium ionic liquid can be easily regenerated, and the extraction capacity was about 94% of the initial one after being used three times.

  18. Fe_3O_4磁粉的合成与结构表征%Preparation of Fe3O4 Nanoparticle by Liquid - phase Coprecipitation

    Institute of Scientific and Technical Information of China (English)

    霍涌前; 陈小利; 王升文; 崔华莉; 王潇

    2012-01-01

    Nanometer magnetite Fe3O4 particles were prepared by chemical co -precipitation, NH3·H2O was cho- sen as precipitating agent and added to the mixed aqueous solution containing ferric and ferrous ions to produce nanometer Fe3O4 particles. Some influence factors on the size were investigated. The phase structure of the particle was measured by XRD test, and the average size was about 28 nm.%采用化学共沉淀法制备纳米磁性Fe3O4粒子。选用NH3.H2O作为沉淀剂,加入到Fe2+和Fe3+的混合盐溶液中,制得了纳米磁性Fe3O4粒子。考察了影响产物粒径的一些实验因素。通过X-Ray谱图证实了产物结构特征,平均粒径在37 nm左右,平均晶粒度只有28 nm左右的均分散。

  19. Electrochemical preparation of polyaniline-polypyrrole solid-phase microextraction coating and its application in the GC determination of several esters.

    Science.gov (United States)

    Zhao, Shasha; Wu, Mian; Zhao, Faqiong; Zeng, Baizhao

    2013-12-15

    A novel polyaniline-polypyrrole (PANI-PPY) composite film coated stainless steel wire was prepared by cyclic voltammetry. Firstly, PANI was electrodeposited on a stainless steel wire from a solution containing 0.1 M aniline and 1M HNO3, after the PANI coating was dried in air PPY was electrodeposited on it from a solution containing 0.1 M pyrrole and 0.1 M p-methylbenzene sulfonic acid. The resulting PANI-PPY fiber showed reticulate structure and had large specific surface area. When it was used for the headspace solid-phase microextraction of several esters (i.e. methyl anthranilate, ethyl-o-aminobenzoate, dimethyl phthalate, methyl laurate, and diethyl phthalate), followed by gas chromatographic determination, it presented higher extraction capability in comparison with PPY and PANI coatings. Under the optimized conditions, the linear ranges were 0.07-300 μg L(-1) and the detection limits were 0.05-0.38 μg L(-1) for different esters. The PANI-PPY fiber also showed high durability, after being used for about 160 times its extraction capacity only changed a little. The proposed method was successfully applied to the determination of these esters in real samples and the recoveries were 90-102%. © 2013 Elsevier B.V. All rights reserved.

  20. Phase composition, microstructure, and mechanical properties of porous Ti-Nb-Zr alloys prepared by a two-step foaming powder metallurgy method.

    Science.gov (United States)

    Rao, X; Chu, C L; Zheng, Y Y

    2014-06-01

    Porous Ti-Nb-Zr alloys with different porosities from 6.06 to 62.8% are prepared by a two-step foaming powder metallurgy method using TiH2, Nb, and Zr powders together with 0 to 50wt% of NH4HCO3. The effects of the amounts of Nb and Zr as well as the sintering temperature (1473 to 1673K) on their phase composition, porosity, morphology, and mechanical characteristics are investigated. By controlling the porosity, Nb and Zr concentrations as well as the sintering temperature, porous Ti-Nb-Zr alloys with different mechanical properties can be obtained, for example, the hardness between 290 and 63HV, the compressive strength between 1530.5 and 73.4MPa, and the elastic modulus between 10.8 and 1.2GPa. The mechanical properties of the sintered porous Ti-Nb-Zr alloys can be tailored to match different requirements for the human bones and are thus potentially useful in the hard tissue implants. Copyright © 2014 Elsevier Ltd. All rights reserved.

  1. High mobility In{sub 2}O{sub 3}:H transparent conductive oxides prepared by atomic layer deposition and solid phase crystallization

    Energy Technology Data Exchange (ETDEWEB)

    Macco, B.; Wu, Y.; Vanhemel, D. [Department of Applied Physics, Eindhoven University of Technology (Netherlands); Kessels, W.M.M. [Department of Applied Physics, Eindhoven University of Technology (Netherlands); Solliance Solar Research, Eindhoven (Netherlands)

    2014-12-01

    The preparation of high-quality In{sub 2}O{sub 3}:H, as transparent conductive oxide (TCO), is demonstrated at low temperatures. Amorphous In{sub 2}O{sub 3}:H films were deposited by atomic layer deposition at 100 C, after which they underwent solid phase crystallization by a short anneal at 200 C. TEM analysis has shown that this approach can yield films with a lateral grain size of a few hundred nm, resulting in electron mobility values as high as 138 cm{sup 2}/V s at a device-relevant carrier density of 1.8 x 10{sup 20} cm{sup -3}. Due to the extremely high electron mobility, the crystallized films simultaneously exhibit a very low resistivity (0.27 mΩ cm) and a negligible free carrier absorption. In conjunction with the low temperature processing, this renders these films ideal candidates for front TCO layers in for example silicon heterojunction solar cells and other sensitive optoelectronic applications. (copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  2. Molecularly imprinted polymer microspheres prepared by Pickering emulsion polymerization for selective solid-phase extraction of eight bisphenols from human urine samples.

    Science.gov (United States)

    Yang, Jiajia; Li, Yun; Wang, Jincheng; Sun, Xiaoli; Cao, Rong; Sun, Hao; Huang, Chaonan; Chen, Jiping

    2015-05-01

    The bisphenol A (BPA) imprinted polymer microspheres were prepared by simple Pickering emulsion polymerization. Compared to traditional bulk polymerization, both high yields of polymer and good control of particle sizes were achieved. The characterization results of scanning electron microscopy and nitrogen adsorption-desorption measurements showed that the obtained molecularly imprinted polymer microsphere (MIPMS) particles possessed regular spherical shape, narrow diameter distribution (30-60 μm), a specific surface area (S(BET)) of 281.26 m(2) g(-1) and a total pore volume (V(t)) of 0.459 cm(3) g(-1). Good specific adsorption capacity for BPA was obtained in the sorption experiment and good class selectivity for BPA and its seven structural analogs (bisphenol F, bisphenol B, bisphenol E, bisphenol AF, bisphenol S, bisphenol AP and bisphenol Z) was demonstrated by the chromatographic evaluation experiment. The MIPMS as solid-phase extraction (SPE) packing material was then evaluated for extraction and clean-up of these bisphenols (BPs) from human urine samples. An accurate and sensitive analytical method based on the MIPMS-SPE coupled with HPLC-DAD has been successfully established for simultaneous determination of eight BPs from human urine samples with detection limits of 1.2-2.2 ng mL(-1). The recoveries of BPs for urine samples at two spiking levels (100 and 500 ng mL(-1) for each BP) were in the range of 81.3-106.7% with RSD values below 8.3%.

  3. Development and validation of a reversed-phase column liquid chromatographic method for the determination of five cephalosporins in pharmaceutical preparations.

    Science.gov (United States)

    Elkady, Ehab F; Abbas, Samah S

    2011-01-01

    A new, simple, rapid, and precise RP-HPLC method has been developed and validated for the determination of five cephalosporins, namely, cefalexin, cefoperazone, ceftriaxone, ceftazidime, and cefepime. The method has been applied successfully for simultaneous determination of cefalexin in a binary mixture with sodium benzoate in a suspension, and cefoperazone in a binary mixture with sulbactam in vials. Chromatographic separation was achieved on a Waters microBondapak C18 column (250 x 4.6 mm id, 10 pm particle size) using the mobile phase monobasic potassium phosphate (50 mM, pH 4.6)-acetonitrile (80 + 20, v/v) with UV detection. A flow rate of 1 mL/min was applied. Linearity, accuracy, and precision were found to be acceptable over the concentration range of 30-300, 3-30, and 15-120 microg/mL for the studied cephalosporins, sodium benzoate, and sulbactam, respectively. The optimized method proved to be specific, robust, and accurate for QC of the cited drugs in their pharmaceutical preparations.

  4. Kinetics of lipase recovery from the aqueous phase of biodiesel production by macroporous resin adsorption and reuse of the adsorbed lipase for biodiesel preparation.

    Science.gov (United States)

    Zhao, Xuebing; Fan, Ming; Zeng, Jing; Du, Wei; Liu, Canming; Liu, Dehua

    2013-04-10

    A commercial macroporous resin (D3520) was screened for lipase recovery by adsorption from the aqueous phase of biodiesel production. The influences of several factors on the adsorption kinetics were investigated. It was found that the kinetic behavior of lipase adsorption by macroporous resin could be well described by pseudo-first-order model. Temperature had no significant effects on lipase adsorption, while resin-to-protein ratio (R) significantly affected both rate constant (k1) and equilibrium adsorption capacity (Qe). No lipase was adsorbed when mixing (shaking) was not performed; however, protein recovery reached 98% after the adsorption was conducted at 200rpm for 5h in a shaker. The presence of methanol and glycerol showed significant negative influence on lipase adsorption kinetics. Particularly, increasing glycerol concentration could dramatically decrease k1 but not impact Qe. Biodiesel was found to dramatically decrease Qe even present at a concentration as low as 0.02%, while k1 was found to increase with biodiesel concentration. The adsorbed lipase showed a relatively stable catalytic activity in tert-butanol system, but poor stability in solvent-free system when used for biodiesel preparation. Oil and biodiesel were also found to adsorb onto resin during transesterification in solvent-free system. Therefore, the resin had to be washed by anhydrous methanol before re-used for lipase recovery.

  5. Preparation and characterization of TiO2 anode film with spinodal phase separation structure in dye-sensitized solar cells

    Science.gov (United States)

    Guli, Mina; Yao, Jianxi; Zhao, Jingyong; Rao, Wangping; Xiao, Li; Tian, Hongxin

    2013-10-01

    Low electronic transmission efficiency and high charge recombination are the existing problems of photoanode film in traditional dye sensitized solar cells (DSSCs). This paper put forward the photoanode TiO2 films with spinodal phase separation structure (SPSS) and continuous TiO2 skeleton which were triggered by the photopolymerization of organic monomers in a photomonomer-inorganic precursor system. The photoanode TiO2 films fabricated by different precursor solution compositions and different coating layers were characterized mainly by scanning electron microscopy (SEM), photocatalysis and photoelectric performance test. The results indicated that, the as-prepared TiO2 anode film with seven coating layers and heat treated at 500 °C showed higher photoelectric conversion efficiency at about 2% than that of other samples with less coating layers and lower heat treatment temperature. The film also showed excellent photocatalytic activity by using methylene blue (MB) dye as a model organic substrate under fluorescent lamp irradiation. It is suggested that the film with SPSS structure has the potential to improve the electronic transmission efficiency and reduce the carrier recombination due to its particular structure, higher surface area, and lack of bottleneck in electronic transmission. It is worth noting that the SPSS structure provides new ideas to develop new photoanode films and further improve the photoelectric conversion performance of the DSSC in future.

  6. Liquid-phase non-thermal plasma-prepared N-doped TiO(2) for azo dye degradation with the catalyst separation system by ceramic membranes.

    Science.gov (United States)

    Cheng, Hsu-Hui; Chen, Shiao-Shing; Cheng, Yi-Wen; Tseng, Wei-Lun; Wang, Yi-Hui

    2010-01-01

    This study strived to improve the photocatalytic activity by using liquid-phase non-thermal plasma (LPNTP) technology for preparing N-doping TiO(2) as well as to separate/recover the N-dope TiO(2) particles by using ceramic ultrafiltration membrane process. The yellow color N-doped TiO(2) photocatalysts, obtained through the LPNTP process, were characterized with UV-Vis spectroscopy, X-ray diffraction (XRD), and electron spectroscopy for chemical analysis (ESCA). The UV-Vis spectrum of N-doped TiO(2) showed that the absorption band was shifted to 439 nm and the band gap was reduced to 2.82 eV. The structure analysis of XRD spectra showed that the peak positions and the crystal structure remained unchanged as anatase after plasma-treating at 13.5 W for 40 min. The photocatalytic activity of N-doped TiO(2) was evaluated by azo dyes under visible light, and 63% of them was degraded after 16 hours in a continuous-flow photocatalytic system. For membrane separation/recover system, the recovery efficiency reached 99.5% after the ultrafiltration had been carried out for 90 min, and the result indicated that the photocatalyst was able to be separated/recovered completely.

  7. Preparation and application of a novel molecularly imprinted solid-phase microextraction monolith for selective enrichment of cholecystokinin neuropeptides in human cerebrospinal fluid.

    Science.gov (United States)

    Ji, Xiang; Li, Dan; Li, Hua

    2015-08-01

    A novel molecularly imprinted polymer (MIP) monolith for highly selective extraction of cholecystokinin (CCK) neuropeptides was prepared in a micropipette tip. The MIPs were synthesized by epitope imprinting technique and the polymerization conditions were investigated and optimized. The synthesized MIPs were characterized by infrared spectroscopy, elemental analyzer and scanning electron microscope. A molecularly imprinted solid-phase microextraction (MI-μ-SPE) method was developed for the extraction of CCK neuropeptides in aqueous solutions. The parameters affecting MI-μ-SPE were optimized. The results indicated that this MIP monolith exhibited specific recognition capability and high enrichment efficiency for CCK neuropeptides. In addition, it showed excellent reusability. This MIP monolith was used for desalting and enrichment of CCK4, CCK5 and CCK8 from human cerebrospinal fluid prior to matrix-assisted laser desorption/ionization time-of-flight mass spectrometry analysis, and the results show that this MIP monolith can be a useful tool for effective purification and highly selective enrichment of multiple homologous CCK neuropeptides in cerebrospinal fluid simultaneously. By employing MI-μ-SPE combined with HPLC-ESI-MS/MS analysis, endogenous CCK4 in human cerebrospinal fluid was quantified.

  8. 相变材料微胶囊的制备及应用%Preparation and application of microcapsules containing phase change materials

    Institute of Scientific and Technical Information of China (English)

    曹虹霞; 李和玉; 张健飞

    2011-01-01

    The phase change microcapsules with n-octadecane as core and melamine-formaldehyde as shell were prepared by in situ polymerization. The fabrics were finished with the microcapsules. The morphology of microcapsules and finished fabrics were characterized by using scanning electron microscopy (SEM); the diameter distributions of the microcapsules were investigated by particle size analyzer; the thermal physical properties of microcapsules and finished fabrics were analyzed by thermal analyzer. The results show that the microcapsule has smaller particle size, narrower particle size distribution and the higher enthalpy. The finished fabrics treated by different technologies have high heat storaging capacity and good thermoregulating capacity.%采用原位聚合法合成了以正十八烷为囊芯、三聚氰胺-甲醛树脂为囊壁的相变材料微胶囊,并用其时棉织物进行了整理.用扫描电镜、激光粒度仪对微胶囊及整理后织物的形貌、粒度进行表征,并时微胶囊及整理后织物的热性能进行了研究,结果表明:微胶囊粒径小,粒径分布窄,具有较高的相变焓;整理后织物具有蓄热调温功能.

  9. 蛋白土负载型复合相变材料的制备与表征%Preparation and Characterization of Opal Loaded Composite Phase-change Materials

    Institute of Scientific and Technical Information of China (English)

    张殿潮; 孔维安; 郑水林; 刘月; 毛俊

    2013-01-01

      采用热熔复混法,以改性蛋白土为基体、石蜡为相变物质,制备出了具有合适相变温度、较大相变潜热的复合储能材料.采用SEM、红外光谱和差示扫描量热 DSC 对复合相变材料的结构和性能进行了表征,结果表明,制备的复合材料相变温度为24.91℃,相变潜热为64.31 J/g,颗粒均匀分布在蛋白土与熔融石蜡构成的基体之中;载体蛋白土和相变材料石蜡之间以分子间作用力的物理吸附结合,得到了稳定的复合相变材料.%Organic phase change materials like paraffin as phase change material, modified opal as carrier, composite phase change material with proper phase change temperature and larger phase change enthalpy is prepared by hot melt complex mixed. The structure and performance of composite phase material are characterized using SEM, infrared spectroscopy and synthesized thermal analyzer DSC. The results show that the phase change temperature of composite phase change materials is 24.91 ℃, and phase change enthalpy is 64.31 J/g. With every part preserved, phase change particles are distributed in the opal/melted paraffin matrix evenly. Stable composite phase change materials are prepared with opal as carrier and paraffin as PCMs, which are bonded with Vander Waals forces in the form of physical adsorption.

  10. Preparation of mixed stationary phase of cellulose and polysiloxane ionic liquid for gas chromatography%纤维素/聚硅氧烷离子液体混合气相色谱固定相的制备

    Institute of Scientific and Technical Information of China (English)

    陈刚; 赵晓洁; 邢钧; 姚玉华; 郑京京

    2014-01-01

    纤维素是液相色谱中应用十分广泛的一类固定相,可是由于涂渍性能不佳,纤维素在气相色谱中的应用鲜有报道。本论文首先通过酯化反应合成了脂溶性较好的三醋酸纤维素( CTA ),然后与自制的聚硅氧烷离子液体( PIL-C12-NTf2)混配,制备了含纤维素的气相色谱固定相( CTA@ PIL-C12-NTf2),并涂渍了毛细管柱。其柱效为3165 plates/m(110℃,萘,k=4.95)。麦氏常数及溶剂化参数模型的测试结果证明,该固定相属中强极性固定相,主要作用力是氢键碱性作用和偶极作用。值得注意的是,引入纤维素可明显改善三取代芳香化合物位置异构体及壬烷( C9)同分异构体的分离选择性。此外,该固定相对正构烷烃、醇、脂肪酸酯及邻苯二甲酸酯等也具有良好的分离选择性。该研究不仅初步展现了纤维素在分离选择性上的特点,而且也为探索纤维素衍生物在气相色谱中的应用提供了一条新的途径。%Cellulose has been widely used to synthesize chiral stationary phases for liquid chro-matography,but it is still absent in the family of stationary phases of gas chromatography due to its poor film-forming property. Based on the unique dissolution characteristic,ionic liquids provide a great chance to solve this problem. In this paper,cellulose triacetate( CTA)was syn-thesized,and then mixed with the home-made polysiloxane ionic liquid(PIL-C12-NTf2)to pro-duce a novel mixed stationary phase(CTA@PIL-C12-NTf2). After that,it was used to prepare a capillary column for gas chromatography. The column efficiency was measured to be 3 165 plates/m(110 ℃,naphthalene,k=4. 95),demonstrating the excellent film-forming capability of this stationary phase,and then the solvation parameter model was employed to find out the interaction parameters of CTA@ PIL-C12-NTf2. In the aspect of selectivity,CTA was firstly demonstrated to be able to improve the

  11. Molecularly imprinted polymer microspheres prepared by Pickering emulsion polymerization for selective solid-phase extraction of eight bisphenols from human urine samples

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Jiajia [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Li, Yun; Wang, Jincheng [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); Sun, Xiaoli; Cao, Rong [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Sun, Hao [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); Department of Chemistry, Liaoning University, Shenyang 110000 (China); Huang, Chaonan [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Chen, Jiping, E-mail: chenjp@dicp.ac.cn [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China)

    2015-05-04

    Highlights: • BPA imprinted polymer microspheres were prepared by Pickering emulsion polymerization. • Regular spherical shape and narrow diameter distribution. • Good specific adsorption capacity for BPA. • Good class-selectivity and clean-up efficiency for bisphenols in human urine under SPE mode. • Good recoveries and sensitivity for bisphenols using the MIPMS-SPE coupled with HPLC-DAD method. - Abstract: The bisphenol A (BPA) imprinted polymer microspheres were prepared by simple Pickering emulsion polymerization. Compared to traditional bulk polymerization, both high yields of polymer and good control of particle sizes were achieved. The characterization results of scanning electron microscopy and nitrogen adsorption–desorption measurements showed that the obtained molecularly imprinted polymer microsphere (MIPMS) particles possessed regular spherical shape, narrow diameter distribution (30–60 μm), a specific surface area (S{sub BET}) of 281.26 m{sup 2} g{sup −1} and a total pore volume (V{sub t}) of 0.459 cm{sup 3} g{sup −1}. Good specific adsorption capacity for BPA was obtained in the sorption experiment and good class selectivity for BPA and its seven structural analogs (bisphenol F, bisphenol B, bisphenol E, bisphenol AF, bisphenol S, bisphenol AP and bisphenol Z) was demonstrated by the chromatographic evaluation experiment. The MIPMS as solid-phase extraction (SPE) packing material was then evaluated for extraction and clean-up of these bisphenols (BPs) from human urine samples. An accurate and sensitive analytical method based on the MIPMS-SPE coupled with HPLC-DAD has been successfully established for simultaneous determination of eight BPs from human urine samples with detection limits of 1.2–2.2 ng mL{sup −1}. The recoveries of BPs for urine samples at two spiking levels (100 and 500 ng mL{sup −1} for each BP) were in the range of 81.3–106.7% with RSD values below 8.3%.

  12. Preparation, phase transition and thermal expansion studies on low-cristobalite type Al 1- xGa xPO 4 ( x=0.0, 0.20, 0.50, 0.80 and 1.00)

    Science.gov (United States)

    Achary, S. N.; Jayakumar, O. D.; Tyagi, A. K.; Kulshresththa, S. K.

    2003-11-01

    The orthorhombic ( α) low-cristobalite type AlPO 4 and GaPO 4 and their solid solutions are prepared by co-precipitation followed by high temperature annealing of the precipitate. The single phasic nature of the products is ascertained by powder XRD at room temperature. The high temperature behavior of these samples is studied by HT-XRD over the temperature range of 25-1000°C. All these compositions undergo an orthorhombic to cubic ( β, high-cristobalite) phase transition at elevated temperature. The unit cell parameters at different temperatures are determined by refining the observed powder diffraction profiles. The phase transition is accompanied by a significant increase in the unit cell volume, leading to the formation of a low dense structure. The variation of unit cell volume with temperature for each composition shows that the orthorhombic phase has a significantly larger thermal expansion than the cubic (high temperature) phase. The high temperature behavior of all the compositions except the GaPO 4 is similar. GaPO 4 undergoes a phase separation to a more stable quartz type phase above 800°C. However, the quartz type phase again transforms to the high cristobalite ( β) phase at 1000°C. Thermal expansions of all these phases are explained in term of the variation of M-O-P angle as a function of temperature.

  13. Preparation of molecularly imprinted solid-phase microextraction fiber for the selective removal and extraction of the antiviral drug abacavir in environmental and biological matrices

    Energy Technology Data Exchange (ETDEWEB)

    Terzopoulou, Zoi [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki (Greece); Papageorgiou, Myrsini [Laboratory of Environmental Pollution Control, Department of Chemistry, Aristotle University of Thessaloniki, GR–541 24, Thessaloniki (Greece); Kyzas, George Z.; Bikiaris, Dimitrios N. [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki (Greece); Lambropoulou, Dimitra A., E-mail: dlambro@chem.auth.gr [Laboratory of Environmental Pollution Control, Department of Chemistry, Aristotle University of Thessaloniki, GR–541 24, Thessaloniki (Greece)

    2016-03-24

    In the present study, a molecularly imprinted solid-phase microextraction fiber (MIP-SPME{sub f}) was synthesized and applied for the selective removal and extraction of the antiviral drug, abacavir (ABA). Morphology and structure characterization of fibers were performed by scanning electron microscopy and Fourier transform infrared spectra, respectively. The effects on the adsorption behavior of the process parameters were studied and the equilibrium data were fitted by the Langmuir, Freundlich and Langmuir-Freundlich models. The maximum adsorption capability (Q{sub max}) was determined by Langmuir- Freundlich model and was 149 mg/g for MIP-SPME{sub f}. In the next step, SPME methodology followed by liquid desorption and liquid chromatography with mass spectrometry (LC/MS) has been developed and evaluated for the determination of the target compound in environmental and biological matrices (surface waters, wastewaters and urine). Parameters that could influence SPME efficiency were investigated. Then, optimization of stirring speed, extraction time and salt content was carried out by using a central composite design (CCD) and response surface methodology (RSM). A quadratic model between dependent and independent variables was built. Under the optimum conditions (extraction time 40 min, stirring rate 650 rpm and salt content 0.3% NaCl w/v) the validated method presented a high sensitivity and selectivity with LODs and LOQs in the range of 10.1–13.6 and 33.3–43.9 ng/L, respectively. The developed method was successfully applied to the analysis of ABA in real samples. The percentage extraction efficiency ranged from 88 to 99% revealing good accuracy and absence of matrix effects. - Highlights: • Preparation of a novel SPME MIP fiber with remarkable recognition properties. • Selective removal and extraction of abacavir from environmental & biological media. • Detailed adsorbent characterization and adsorption studies. • Successful application of

  14. Zirconium basic carbonate preparation by low-temperature solid-phase reaction method%低温固相反应法制备碱式碳酸锆

    Institute of Scientific and Technical Information of China (English)

    邱才华; 罗方承; 黄可龙

    2013-01-01

    Sodium zirconium basic carbonate precursor is prepared using zirconyl chloride and sodium carbonate as raw materials by low-temperature solid-phase reaction. Zirconium basic carbonate is then produced by adding dilute hydrochloric acid and cleaning on the precursor. This paper studies the effects of milling time and milling speed on the product granularity by performing infrared spectroscopy on the zirconium basic carbonate. The effect of acid pH degree on the product impurity content is also studied. The results show that the average particle size of zirconium basic carbonate products is around 11 μm with characteristics of uniform particle size distribution, good dispersion, strong activity and high purity under the optimal technical conditions (zirconium beads milling, milling speed with 150 r/min, milling time for 2 h, acid pH value amounting to 3.9~4.1).%  采用氧氯化锆和碳酸钠为原料进行低温固相反应,得到碱式碳酸锆钠前驱物,前驱物经过加稀盐酸和除杂后得到碱式碳酸锆.对碱式碳酸锆进行了红外光谱分析,并通过条件实验,研究了球磨时间、球磨转速对产物粒度和调酸pH对产物杂质含量的影响.结果表明:在对原料采用锆珠球磨、球磨转速150 r/min、球磨时间为2 h,对前驱物调酸除杂pH值稳定在3.9~4.1的最佳工艺条件下,制备的碱式碳酸锆产品平均粒度大约11μm,粒度分布均匀、分散性好、活性强、纯度高.

  15. Preparation of Graphite Foam/Eutectic Salt Composite Phase Change Materials%石墨泡沫/共晶盐复合相变材料制备

    Institute of Scientific and Technical Information of China (English)

    罗志军; 郭茶秀

    2015-01-01

    选择KNO3/NaNO3二元体系按照质量比4:6制备共晶盐,对共晶盐进行了熔点及熔化潜热的测量;将石墨泡沫这一新型材料作为强化基体,共晶盐作为相变材料(PCM),采用熔融浸渗法制备了适用于太阳能热发电系统储能装置的石墨泡沫/共晶盐复合相变材料.采用扫描电镜对复合相变材料表面的微观结构进行了表征,并对其熔点、潜热、等效导热系数等热物性参数进行了测试.结果表明:共晶盐与石墨泡沫复合效果比较理想;复合前后共晶盐的熔点和潜热几乎没有发生变化;复合相变材料的等效导热系数得到了显著提升,石墨泡沫对相变材料起到了导热强化作用,满足高温蓄热的要求.%Eutectic salt (KNO3/NaNO3) with the mass ratio of 4:6 was firstly prepared then the melting point and latent heat of eutectic salt were obtained by experiments.Next, graphite foam/eutectic salt composite PCM was fabricated successfully by melting impregnation method. In this material, graphite foam and eutectic salt were treated as strengthening matrix and PCM respectively. This kind of composite PCM was suitable for energy storage device in solar thermal power generation system.The microstructure of the composite phase change material was characterized with scanning electron microscopy. The thermo-physical properties of composite PCM including melting point, latent heat and effective thermal conductivity were acquired by DSC test and laser flash technique.The results showed that:the composite effect of eutectic salt and graphite foam was ideal. The melting point of the eutectic salt and latent heat did not change after the impregnation. Composite PCM with high effective thermal conductivity, completely meet the requirements of high temperature heat storage.

  16. Preparation of a sample with a single MgH2 phase by horizontal ball milling and the first hydriding reaction of 90 wt% Mg-10 wt% MgH2

    Science.gov (United States)

    Hong, Seong-Hyeon; Song, Myoung Youp

    2015-03-01

    In order to prepare an additive-free sample with a single MgH2 phase, 90 wt% Mg-10 wt% MgH2 (named 90Mg-10MgH2) was milled under a hydrogen atmosphere in a horizontal ball mill, and then hydrided. The hydrogen absorption and desorption properties of the prepared samples were investigated, and compared with those of milled pure Mg and purchased MgH2. X-ray diffraction analysis, measurement of specific BET surface areas, and observation of the prepared samples by scanning electron microscope were performed. The 90Mg-10MgH2 sample after hydriding-dehydriding cycling had small and large particles with fine particles on their surfaces, and had much finer particles and more defects than the milled pure Mg sample after hydridingdehydriding cycling. The specific BET surface areas of the milled Mg and 90Mg-10MgH2 were measured as 7.81 and 99.81 m2/g, respectively. A sample that had almost a single MgH2 phase could be prepared by horizontal ball milling and the first hydriding reaction of 90Mg-10MgH2. 90Mg-10MgH2 released 5.82 wt% H for about 70 min, while unmilled MgH2 (Aldrich) released 6.04 wt% H for about 100 min, at 648 K.

  17. Pressure-driven one-step solid phase-based on-chip sample preparation on a microfabricated plastic device and integration with flow-through polymerase chain reaction (PCR).

    Science.gov (United States)

    Tran, Hong Hanh; Trinh, Kieu The Loan; Lee, Nae Yoon

    2013-10-01

    In this study, we fabricate a monolithic poly(methylmethacrylate) (PMMA) microdevice on which solid phase-based DNA preparation and flow-through polymerase chain reaction (PCR) units were functionally integrated for one-step sample preparation and amplification operated by pressure. Chelex resin, which is used as a solid support for DNA preparation, can capture denatured proteins but releases DNA, and the purified DNA can then be used as a template in a subsequent amplification process. Using the PMMA microdevices, DNA was successfully purified from both Escherichia coli and human hair sample, and the plasmid vector inserted in E. coli and the D1S80 locus in human genomic DNA were successfully amplified from on-chip purified E. coli and human hair samples. Furthermore, the integration potential of the proposed sample preparation and flow-through PCR units was successfully demonstrate on a monolithic PMMA microdevice with a seamless flow, which could pave the way for a pressure-driven, simple one-step sample preparation and amplification with greatly decreased manufacture cost and enhanced device disposability.

  18. 微胶囊相变材料制备技术的研究进展%Progress in Study on the Preparation Technology of Microencapsulated Phase Change Material

    Institute of Scientific and Technical Information of China (English)

    王刚; 秦立翠; 姜艳

    2012-01-01

    Microencapsulated phase change materials (MEPCM) is a kind of composite material with core-shell structure constructed by coating a polymer layer with stable performance on the surface of solid-liquid phase change material by microencapsulation technology. The classification of phase change materials, working principle of microencapsulated phase change material is presented, and several preparation methods for microcapsule are introduced emphatically, including the interfacial polymerization, in-situ polymerization, complex coacervation method, solvent evaporation method and condensed phase separation method. The development trend of microencapsulation technology is proposed.%微胶囊相变材料( Microencapsulated Phase Change Material,MEPCM)是应用微胶囊技术在固液相变材料表面包覆一层性能稳定的高分子膜,而构成的具有核壳结构的复合材料.系统地讲述了相变材料的分类,微胶囊相变材料的工作原理,并重点介绍了几种微胶囊的制备方法,包括界面聚合法、原位聚合法、复凝聚法、溶剂挥发法、凝聚相分离法等,并提出了微胶囊技术今后的发展方向.

  19. Preparation and application of methylcalix[4]resorcinarene-bonded silica particles as chiral stationary phase in high-performance liquid chromatography.

    Science.gov (United States)

    Tan, Huey Min; Soh, Shu Fang; Zhao, Jia; Yong, E L; Gong, Yinhan

    2011-01-01

    Two new types of methylcalix[4]resorcinarene-bonded stationary phases, (3-(C-methylcalix[4]resorcinarene)-2-hydroxypropoxy)-propylsilyl-appended silica particles (MCR-HPS) and bromoacetate-substituted MCR-HPS particles (BAMCR-HPS), have been synthesized and used as chiral stationary phases for high-performance liquid chromatography (HPLC) for the first time. The synthetic stationary phases are characterized by means of elemental analysis and Fourier-transform infrared spectroscopy. The chromatographic behavior of MCR-HPS and BAMCR-HPS was studied with several disubstituted benzenes and some chiral drug compounds under both normal phase and reversed-phase conditions. The results show that MCR-HPS has excellent selectivity for the separation of aromatic positional isomers and BAMCR-HPS exhibits excellent performance for separation of enantiomers of chiral compounds.

  20. Preparation and characterization of cross-linking PEG/MDI/PE copolymer as solid-solid phase change heat storage material

    Energy Technology Data Exchange (ETDEWEB)

    Li, Wei-Dong [Key Laboratory of Cellulose and Lignocellulosics Chemistry, Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou 510650 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100039 (China); Ding, En-Yong [Key Laboratory of Cellulose and Lignocellulosics Chemistry, Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou 510650 (China)

    2007-05-23

    Phase change materials (PCMs) are a series of functional materials with storing and releasing energy properties. PCMs can impact small environment around them through storing and releasing energy during phase change process. Phase change latent heat of PCMs has two main characters: one is high enthalpy and capacity of per unit volume and the other is that the temperature over phase change process keeps constant or changes slightly. PCMs have been widely used in lots of fields such as solar energy storing, smart housing, thermo-regulated fibers and agricultural greenhouse. In this article, a novel solid-solid phase change heat storage material was synthesized via the two-step condensation reaction of high molecule weight polyethylene glycol (PEG10000) with pentaerythritol (PE) and 4,4'-diphenylmethane diisocyanate (MDI). To characterize the resulting product in comparison with pristine PEG10000, Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), thermogravimetric analyses (TGA), polarization optical microscopy (POM) and wide-angle X-ray diffraction (WAXD) measurements were employed to investigate their ingredients, thermal properties and crystalline behaviors. The results indicated that the cross-linking PCM showed typical solid-solid phase transition property, and its phase change enthalpy and crystallinity reached 152.97 kJ/kg and 81.76%, respectively. (author)

  1. The Phase Diagram of MgB2 Superconductor and its Guiding to Thin Film Preparation%MgB2超导体的相图及其对薄膜制备的指导作用

    Institute of Scientific and Technical Information of China (English)

    汪怀蓉; 李良荣; 张荣芬; 李绪诚; 虞苏青

    2012-01-01

    MgB2 is well fitted for the implementation of Josephson junction, and is useful in superconductor electrics. Preparation of high-quality MgB2 thin film is critical. The Mg-B/Mg-B-0 thermodynamics phase diagram and its phase relation has important value in preparation for high-quality MgB2 film. In this paper, some aspects of MgB2 thin film preparation were involved, including the current progress of superconducting MgB2, the Mg-B/ Mg-B-0 thermodynamics phase diagram and its phase relation, the information mechanism of MgO phase in oxygen-rich region and its influence to MgB2 thin film growing. Then, the guidance to MgB2 film of Mg-B/Mg-B-O thermodynamics phase diagram was discussed in detail. At last, the HPCVD( Hybrid Physical Chemical Vapor Deposition)in-situ thin film fabrication methods under the guiding of MgB2 phase diagram was proposed.%MgB2适合于制备约瑟夫森结,在超导电子学领域有很好的应用前景.制备高质量的MgB2薄膜至关重要,应用Mg-B/Mg-B-O体系的相图指导MgB2薄膜生长意义重大.总结MgB2相体系及相关系,详细对比分析Mg-B/Mg-B-O体系的热力学相图,总结分析富氧区杂项MgO的生成机理及其对MgB2薄膜质量和性能的影响,研究分析有氧体系下Mg-B/Mg-B-O热力学相图对MgB2薄膜材料制备生长的指导意义,探讨HPCVD环境下采用原位生长技术制备MgB2超导薄膜时热力学相图的指导作用及相关制备工艺.

  2. Phase-space geometry of the generalized Langevin equation.

    Science.gov (United States)

    Bartsch, Thomas

    2009-09-28

    The generalized Langevin equation is widely used to model the influence of a heat bath upon a reactive system. This equation will here be studied from a geometric point of view. A dynamical phase space that represents all possible states of the system will be constructed, the generalized Langevin equation will be formally rewritten as a pair of coupled ordinary differential equations, and the fundamental geometric structures in phase space will be described. It will be shown that the phase space itself and its geometric structure depend critically on the preparation of the system: A system that is assumed to have been in existence forever has a larger phase space with a simpler structure than a system that is prepared at a finite time. These differences persist even in the long-time limit, where one might expect the details of preparation to become irrelevant.

  3. Influence of Mobile Phase Composition on the Enantioseparation of Methoxyl Flavanones with Self-prepared CDMPC Column and Chiral Recognition Mechanism

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    The influence of different alcohol modifiers in mobile phase on the chiral separation of 4`-methoxyl flavanone, 5-methoxyl flavanone and 6-methoxyl flavanone on cellulose tris (3, 5-dimethylphenylcarbamate) (CDMPC) column was studied and the chiral recognition mechanism was discussed. Using hexane-tert-butanol (1.31 mol L-1) as the mobile phase, those three methoxyl flavanones were excellently separated on CDMPC chiral column.

  4. Phase development and electrical properties of Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-PbTiO{sub 3} ceramics prepared by partial oxalate route

    Energy Technology Data Exchange (ETDEWEB)

    Qian, Kun; Fang, Bijun; Du, Qingbo [School of Materials Science and Engineering, Changzhou University, Changzhou, Jiangsu (China); Ding, Jianning [School of Materials Science and Engineering, Changzhou University, Changzhou, Jiangsu (China); School of Material Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu (China); Zhao, Xiangyong; Luo, Haosu [Key Laboratory of Inorganic Function Material and Device, Chinese Academy of Sciences, Shanghai (China)

    2013-06-15

    (1 - x)Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-xPbTiO{sub 3} (PMN-PT, x = 0.2-0.4) ferroelectric (FE) ceramics were prepared by the partial oxalate route. The synthesized PMN-PT ceramics exhibit high density and densified microstructure although slight content of pyrochlore phase impurity exists. With the increase of PbTiO{sub 3} (PT) content, the phase structure of the PMN-PT ceramics changes gradually from rhombohedral perovskite structure, across the morphotropic phase boundary (MPB) composition and to tetragonal perovskite structure. The FE structural phase transition of PMN-PT changes gradually from the diffused ferroelectric phase transition (FPT) of typical relaxor FEs to nearly first-order FPT of normal FEs, confirmed by dielectric and FE properties measurements. The PMN-PT ceramics exhibit excellent dielectric and piezoelectric properties, and fully developed and saturated P-E hysteresis loops, in which the MPB effects are clearly shown by these electrical properties. The MPB composition of the PMN-PT system is determined locating at x = 0.31-0.33 by XRD measurement and electrical properties measurements. (copyright 2013 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  5. Effect of the preparation method of support on the aqueous phase reforming of ethylene glycol over 2 wt% Pt/Ce0.15Zr0.85O2 catalysts.

    Science.gov (United States)

    Kim, Jung-Hyun; Jeong, Kwang-Eun; Kim, Tae-Wan; Chae, Ho-Jeong; Jeong, Soon-Yong; Kim, Chul-Ung; Lee, Kwan-Young

    2013-08-01

    The effect of catalyst support on the aqueous phase reforming of ethylene glycol over supported 2 wt% Pt/Ce0.15Zr0.85O2 catalysts have been investigated. Various types of Ce0.15Zr0.85O2 mixed oxides were prepared by hydrothermal precipitation (CZH), modified precipitation (CZM), co-precipitation (CZC), sol-gel (CZS) methods, respectively. Catalysts were characterized by XRD, N2 sorption analysis, and cyclohexane dehydration for relative metal dispersion. The support effect on the activity of 2 wt% Pt/Ce0.15Zr0.85O2 catalysts with different preparation method was given as follows: CZH production rate and hydrogen yield increased in proportion to the reaction temperature and corresponding system pressure, whereas WHSV did not affect.

  6. Preparation of nanosize Cu-ZnO/Al{sub 2}O{sub 3} catalyst for methanol synthesis by phase transfer with metal surfactant. 2: Effect of additives and chain length of surfactant

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Z.; Chen, S.; Peng, S. [Chinese Academy of Science, Taiyuan, Shanxi (China). Inst. of Coal Chemistry

    1996-09-25

    Nanosize Cu-ZnO/Al{sub 2}O{sub 3} catalysts for methanol synthesis were prepared by the metal surfactant phase transfer technique. The effects of chain length of surfactant and additives were studied. It was found that the longer the organic chain of surfactant, the more stable the sol particles and the larger the surface area of catalyst. The decomposition temperature of surfactants with longer chains was also higher. For the preparation of Cu-ZnO/Al{sub 2}O{sub 3} catalyst, the surfactant organic chain should not be longer than 11 carbon atoms. A synergist could be used to improve surfactant efficiency. A stabilizing agent was used to strength the stability of sol particles in water. The time needed for oil-water separation was reduced markedly by using a demulsifying agent. The optimal mole ratios of synergist, stabilizing agent, and demulsifying agent to surfactant were, respectively, 0.6, 0.6, and 1.

  7. Preparation of a weak anion exchange/hydrophobic interaction dual-function mixed-mode chromatography stationary phase for protein separation using click chemistry.

    Science.gov (United States)

    Zhao, Kailou; Yang, Fan; Xia, Hongjun; Wang, Fei; Song, Qingguo; Bai, Quan

    2015-03-01

    In this study, 3-diethylamino-1-propyne was covalently bonded to the azide-silica by a click reaction to obtain a novel dual-function mixed-mode chromatography stationary phase for protein separation with a ligand containing tertiary amine and two ethyl groups capable of electrostatic and hydrophobic interaction functionalities, which can display hydrophobic interaction chromatography character in a high-salt-concentration mobile phase and weak anion exchange character in a low-salt-concentration mobile phase employed for protein separation. As a result, it can be employed to separate proteins with weak anion exchange and hydrophobic interaction modes, respectively. The resolution and selectivity of the stationary phase were evaluated in both hydrophobic interaction and ion exchange modes with standard proteins, respectively, which can be comparable to that of conventional weak anion exchange and hydrophobic interaction chromatography columns. Therefore, the synthesized weak anion exchange/hydrophobic interaction dual-function mixed-mode chromatography column can be used to replace two corresponding conventional weak anion exchange and hydrophobic interaction chromatography columns to separate proteins. Based on this mixed-mode chromatography stationary phase, a new off-line two-dimensional liquid chromatography technology using only a single dual-function mixed-mode chromatography column was developed. Nine kinds of tested proteins can be separated completely using the developed method within 2.0 h.

  8. Combined supercritical fluid extraction/solid-phase extraction with octadecylsilane cartridges as a sample preparation technique for the ultratrace analysis of a drug metabolite in plasma.

    Science.gov (United States)

    Liu, H; Cooper, L M; Raynie, D E; Pinkston, J D; Wehmeyer, K R

    1992-04-01

    Supercritical fluid extraction was coupled with solid-phase extraction using octadecylsilane cartridges for the selective isolation of ultratrace levels of a drug metabolite, mebeverine alcohol, from plasma. Plasma was directly applied to the extraction cartridge, the cartridge was washed to remove protein and then extracted under supercritical conditions using CO2/5% methanol. The effluent from the extraction cell was bubbled through a small volume of 2-propanol to trap the extracted mebeverine alcohol. The effects of extraction pressure and temperature on analyte recovery were examined. The absolute recovery, selectivity, precision, and accuracy of the combined supercritical fluid extraction/solid-phase extraction approach were compared to those of conventional solid-phase extraction using gas chromatography/mass spectrometry in the selected-ion monitoring mode. Mebeverine alcohol was used as a model compound, and dog plasma was employed as the biological matrix for these studies.

  9. Complete suppression of metastable phase and significant enhancement of magnetic properties of B-rich PrFeB nanocomposites prepared by devitrifying amorphous ribbons

    Science.gov (United States)

    Zhang, W. Y.; Chiu, C. H.; Zhang, L. C.; Biswas, K.; Ehrenberg, H.; Chang, W. C.; Eckert, J.

    2007-01-01

    The effect of refractory element addition on phase transformation, crystallization behavior and magnetic properties of Pr 8.5Fe 81.5B 10 (addition-free) and Pr 8.5Fe 81.5M 2B 10 (M=V, Cr, Nb, Zr, Ti) ribbons has been investigated. The annealed addition-free ribbon as well as the samples with V or Cr additions are mainly composed of the metastable Pr 2Fe 23B 3 phase, whereas annealed ribbons with Nb, Zr or Ti additions primarily consist of Pr 2Fe 14B and a minor amount of Fe 3B/boride. The complete suppression of the metastable Pr 2Fe 23B 3 phase due to Nb, Zr or Ti additions leads to a significant enhancement of the magnetic properties. For example, the remanence, the coercivity and the energy product are remarkably increased from 2.5 kG, 0.4 kOe and 0.2 MG Oe for the addition-free material to 9.2 kG, 4.7 kOe and 7.6 MG Oe for the specimens with Nb addition. The successful elimination of the metastable Pr 2Fe 23B 3 phase is believed to profit from two factors: (a) Nb, Zr or Ti atoms substitute the Pr site, comparatively increase the Pr content, and thus inhibit the nucleation of Pr-lean Pr 2Fe 23B 3 phases, and (b) the formation of Nb, Zr, or Ti borides consumes some part of B, which hinders the generation of the B-rich Pr 2Fe 23B 3 phase.

  10. Complete suppression of metastable phase and significant enhancement of magnetic properties of B-rich PrFeB nanocomposites prepared by devitrifying amorphous ribbons

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, W.Y. [FG Physikalische Metallkunde, FB 11 Material- und Geowissenschaften, Technische Universitaet Darmstadt, Petersenstrasse 23, D-64287 Darmstadt (Germany)]. E-mail: wyzhang2005@yahoo.com; Chiu, C.H. [Department of Physics, National Chung Cheng University, 168, San-Hsing, Min-Hsiung, Chia-Yi 621, Taiwan (China); Zhang, L.C. [FG Physikalische Metallkunde, FB 11 Material- und Geowissenschaften, Technische Universitaet Darmstadt, Petersenstrasse 23, D-64287 Darmstadt (Germany); Biswas, K. [Leibniz-Institut fuer Festkoerper- und Werkstoffforschung Dresden, Helmholtzstr. 20, D-01069 Dresden (Germany); Ehrenberg, H. [Institute for Materials Science, Darmstadt University of Technology, Petersenstrasse 23, D-64287 Darmstadt (Germany); Chang, W.C. [Department of Physics, National Chung Cheng University, 168, San-Hsing, Min-Hsiung, Chia-Yi 621, Taiwan (China); Eckert, J. [FG Physikalische Metallkunde, FB 11 Material- und Geowissenschaften, Technische Universitaet Darmstadt, Petersenstrasse 23, D-64287 Darmstadt (Germany)

    2007-01-15

    The effect of refractory element addition on phase transformation, crystallization behavior and magnetic properties of Pr{sub 8.5}Fe{sub 81.5}B{sub 10} (addition-free) and Pr{sub 8.5}Fe{sub 81.5}M{sub 2}B{sub 10} (M=V, Cr, Nb, Zr, Ti) ribbons has been investigated. The annealed addition-free ribbon as well as the samples with V or Cr additions are mainly composed of the metastable Pr{sub 2}Fe{sub 23}B{sub 3} phase, whereas annealed ribbons with Nb, Zr or Ti additions primarily consist of Pr{sub 2}Fe{sub 14}B and a minor amount of Fe{sub 3}B/boride. The complete suppression of the metastable Pr{sub 2}Fe{sub 23}B{sub 3} phase due to Nb, Zr or Ti additions leads to a significant enhancement of the magnetic properties. For example, the remanence, the coercivity and the energy product are remarkably increased from 2.5 kG, 0.4 kOe and 0.2 MG Oe for the addition-free material to 9.2 kG, 4.7 kOe and 7.6 MG Oe for the specimens with Nb addition. The successful elimination of the metastable Pr{sub 2}Fe{sub 23}B{sub 3} phase is believed to profit from two factors: (a) Nb, Zr or Ti atoms substitute the Pr site, comparatively increase the Pr content, and thus inhibit the nucleation of Pr-lean Pr{sub 2}Fe{sub 23}B{sub 3} phases, and (b) the formation of Nb, Zr, or Ti borides consumes some part of B, which hinders the generation of the B-rich Pr{sub 2}Fe{sub 23}B{sub 3} phase.

  11. Marc Treib: Representing Landscape Architecture

    DEFF Research Database (Denmark)

    Braae, Ellen Marie

    2008-01-01

    The editor of Representing Landscape Architecture, Marc Treib, argues that there is good reason to evaluate the standard practices of representation that landscape architects have been using for so long. In the rush to the promised land of computer design these practices are now in danger of being...... left by the wayside. The 14 often both fitting and well crafted contributions of this publication offer an approach to how landscape architecture has been and is currently represented; in the design study, in presentation, in criticism, and in the creation of landscape architecture....

  12. Representative process sampling - in practice

    DEFF Research Database (Denmark)

    Esbensen, Kim; Friis-Pedersen, Hans Henrik; Julius, Lars Petersen

    2007-01-01

    Didactic data sets representing a range of real-world processes are used to illustrate "how to do" representative process sampling and process characterisation. The selected process data lead to diverse variogram expressions with different systematics (no range vs. important ranges; trends and....../or periodicity; different nugget effects and process variations ranging from less than one lag to full variogram lag). Variogram data analysis leads to a fundamental decomposition into 0-D sampling vs. 1-D process variances, based on the three principal variogram parameters: range, sill and nugget effect...

  13. Advanced methods for preparation and characterization of infrared detector materials. [crystallization and phase diagrams of Hg sub 1-x Cd sub x Te

    Science.gov (United States)

    Lehoczy, S. L.

    1979-01-01

    Crystal growth of Hg sub 1-x Cd sub x Te and density measurements of ingot slices are discussed. Radial compositional variations are evaluated from the results of infrared transmission edge mapping. The pseudo-binary HgTe-CdTe phase diagram is examined with reference to differential thermal analysis measurements. The phase equilibria calculations, based on the 'regular association solution' theory (R.A.S.) are explained and, using the obtained R.A.S. parameters, the activities of Hg, Cd, and Te vapors and their partial pressures over the pseudo-binary melt are calculated.

  14. Yucca Mountain Climate Technical Support Representative

    Energy Technology Data Exchange (ETDEWEB)

    Sharpe, Saxon E

    2007-10-23

    The primary objective of Project Activity ORD-FY04-012, “Yucca Mountain Climate Technical Support Representative,” was to provide the Office of Civilian Radioactive Waste Management (OCRWM) with expertise on past, present, and future climate scenarios and to support the technical elements of the Yucca Mountain Project (YMP) climate program. The Climate Technical Support Representative was to explain, defend, and interpret the YMP climate program to the various audiences during Site Recommendation and License Application. This technical support representative was to support DOE management in the preparation and review of documents, and to participate in comment response for the Final Environmental Impact Statement, the Site Recommendation Hearings, the NRC Sufficiency Comments, and other forums as designated by DOE management. Because the activity was terminated 12 months early and experience a 27% reduction in budget, it was not possible to complete all components of the tasks as originally envisioned. Activities not completed include the qualification of climate datasets and the production of a qualified technical report. The following final report is an unqualified summary of the activities that were completed given the reduced time and funding.

  15. Diversity and representativeness: two key factors

    CERN Multimedia

    Staff Association

    2013-01-01

    In the past few weeks many of you have filled out the questionnaire for preparing the upcoming Five-yearly review. Similarly, Staff Association members have elected their delegates to the Staff Council for the coming two years. Once again we would like to thank all those who have taken the time and effort to make their voice heard on these two occasions. Elections to the Staff Council Below we publish the new Staff Council with its forty delegates who will represent in 2014 and 2015 all CERN staff in the discussions with Management and Member States in the various bodies and committees. Therefore it is important that the Staff Council represents as far as possible the diversity of the CERN population. By construction, the election process with its electoral colleges and two-step voting procedure guarantees that all Departments, even the small ones, and the various staff categories are correctly represented. Figure 1 shows the participation rate in the elections. The average rate is just above 52 %, with ...

  16. Preparation of detergent-lipase complexes utilizing water-soluble amphiphiles in single aqueous phase and catalysis of transesterifications in homogeneous organic solvents.

    Science.gov (United States)

    Mine, Y; Fukunaga, K; Maruoka, N; Nakao, K; Sugimura, Y

    2000-01-01

    A novel method of preparing detergent-enzyme complexes that can be employed in organic media was developed utilizing newly synthesized water-soluble nonionic gemini-type detergents, N,N-bis(3-D-gluconamidopropyl)-3-(dialkyl-L-glutamatecarbonyl)propanamides (BIG2CnCA: n = 10,12,14,16,18) and N,N-bis(3-D-lactonamidopropyl)-3-(dialkyl-L-glutamatecarbonyl)propanamides (BIL2CnCA: n = 16,18), and nonionic twin-headed detergents, N,N-bis(3-D-gluconamidopropyl)alkanamides (BIG1Cn: n = 12,14,16,18,delta9). This method simply entails mixing a selected enzyme with an appropriate detergent in an aqueous solution followed by lyophilization, and it offers the advantages of enhanced enzymatic activity in organic solvents and eliminates both enzyme loss and the necessity for an organic solvent in the preparation stage. Using various modified lipases originating from Aspergillus niger (Lipase A), Candida rugosa (Lipase C), Pseudomonas cepacia (Lipase P), and porcine pancreas (PPL), prepared using the novel method and detergents, including conventional synthesized nonionic detergents such as dialkyl N-D-glucona-L-glutamates (2CnGE: n = 12,18delta9) and octanoyl-N-methylglucamide (MEGA-8), enantioselective transesterifications of 6-methyl-5-hepten-2-ol (sulcatol) and 2,2-dimethyl-1,3-dioxolane-4-methanol (solketal) with a vinyl or isopropenyl carboxylate were carried out in an organic solvent. The modified lipase activity was influenced by both the lipases and the structure of the detergents. The value for the hydrophile-lipophile balance (HLB) of the detergent provided a means of correlating the structure and the obtained modified lipase activity. For detergents of the same class with a HLB value of approximately 9 and 12, the highest activity was obtained for Lipase A and Lipase P, and Lipase C and PPL, respectively. Among detergents of the same HLB value tested, the gemini-type detergents possessing the most bulky head and tail were most effective as a modifier for lipases of all

  17. A Study of Curriculums for Occupational Preparation and Education (Scope Program: Phase I). A Systems Model for Instructional Design and Management. Incidental Report #3.

    Science.gov (United States)

    Tuckman, Bruce W.

    A systems model for the design and management of instruction in occupational fields is described. The model is broken down into these phases: (1) analysis, in which occupational tasks are specified via task analysis, tasks are restated as behavioral objectives and a sequence is specified for the objectives, (2) synthesis, in which instructional…

  18. A Lab on a chip device for rapid identification of Avian Influenza virus by on-chip sample preparation and solid phase PCR

    DEFF Research Database (Denmark)

    Yi, Sun; Dhumpa, Raghuram; Bang, Dang Duong

    2009-01-01

    In this paper, we describe a novel lab-on-a-chip device for fast AIV screening by integrating DNA microarray-based solid phase PCR on microchip. The device can handle viral samples in an automatic way. Moreover, multiplex PCR and sequence detection are done in one-step, which greatly simplifies...

  19. Preparation of aqueous two-phase systems composed of two pH-response polymers and liquid-liquid extraction of demeclocycline.

    Science.gov (United States)

    Yan, Bo; Cao, Xuejun

    2012-07-06

    Aqueous two-phase systems have potential applications for separation and purification of bioproducts in bio-industry. However, a key problem is the recovery of the polymers forming aqueous two-phase systems. In this study, two novel random copolymers (P(ADB) and P(ADBA)) were synthesized using acrylic acid, dimethylamino-ethyl methacrylate, butyl methacrylate and allyl alcohol as monomers and used to form pH response aqueous two-phase systems. The recoveries of P(ADB) and P(ADBA) are 97.18% and 98.87% and the pI of P(ADB) and P(ADBA) are 2.79 and 4.01, respectively. Demeclocycline was partitioned in the P(ADB)/P(ADBA) aqueous two-phase systems and the partition coefficient reached 0.085, in the presence of MgSO₄ (60 mmol/L) at pH 5.28. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. A Lab on a chip device for rapid identification of Avian Influenza virus by on-chip sample preparation and solid phase PCR

    DEFF Research Database (Denmark)

    Yi, Sun; Dhumpa, Raghuram; Bang, Dang Duong

    2009-01-01

    In this paper, we describe a novel lab-on-a-chip device for fast AIV screening by integrating DNA microarray-based solid phase PCR on microchip. The device can handle viral samples in an automatic way. Moreover, multiplex PCR and sequence detection are done in one-step, which greatly simplifies t...

  1. Development of a nursing intervention to prepare frail older patients for cardiac surgery (the PREDOCS programme), following phase one of the guidelines of the Medical Research Council.

    Science.gov (United States)

    Ettema, Roelof G A; Hoogendoorn, Marga E; Kalkman, Cor J; Schuurmans, Marieke J

    2014-12-01

    In older patients undergoing elective cardiac surgery, the timely identification and preparation of patients at risk for frequent postoperative hospital complications provide opportunities to reduce the risk of these complications. We developed an evidence-based, multi-component nursing intervention (Prevention of Decline in Older Cardiac Surgery Patients; the PREDOCS programme) for application in the preadmission period to improve patients' physical and psychosocial condition to reduce their risk of postoperative complications. This paper describes in detail the process used to design and develop this multi-component intervention. In a team of researchers, experts, cardiac surgeons, registered cardiac surgery nurses, and patients, the revised guidelines for developing and evaluating complex interventions of the Medical Research Council (MRC) were followed, including identifying existing evidence, identifying and developing theory and modelling the process and outcomes. Additionally, the criteria for reporting the development of complex interventions in healthcare (CReDECI) were followed. The intervention is administered during a consultation by the nurse two to four weeks before the surgery procedure. The consultation includes three parts: a general part for all patients, a second part in which patients with an increased risk are identified, and a third part in which selected patients are informed about how to prepare themselves for the hospital admission to reduce their risk. Following the MRC guidelines, an extended, stepwise, multi-method procedure was used to develop the multi-component nursing intervention to prepare older patients for cardiac surgery, creating transparency in the assumed working mechanisms. Additionally, a detailed description of the intervention is provided. © The European Society of Cardiology 2013.

  2. Advanced fluidic handling and use of two-phase flow for high throughput structural investigation of proteins on a microfluidic sample preparation platform

    DEFF Research Database (Denmark)

    Lafleur, Josiane P.; Snakenborg, Detlef; Møller, M.

    2010-01-01

    Research on the structure of proteins can bring forth a wealth of information about biological function and can be used to better understand the processes in living cells. This paper reports a new microfluidic sample preparation system for the structural investigation of proteins by Small Angle X......-ray Scattering (SAXS). The system includes hardware and software features for precise fluidic control, synchrotron beamline control, UV absorbance measurements and automated data analysis. The precise fluidic handling capabilities are used to transport and precisely position samples as small as 500 n...

  3. Characterizations of Tb:Zn2SiO4 films on silicon wafer prepared by sol-gel dip-coating and solid-phase reaction

    Institute of Scientific and Technical Information of China (English)

    Ji Zhen-Guo; Zhao Shi-Chao; Xiang Yin; Song Yong-Liang; Ye Zhi-Zhen

    2004-01-01

    Terbium-doped Zn2SiO4 films were successfully prepared on Si wafers by a simple sol-gel dip-coating and solidphase reaction method of ZnO and SiO2. X-ray diffraction (XRD) and UV-Vis absorption results revealed that films processed below 850℃ were ZnO in wurzite structure, and films processed above 850℃ were Zn2SiO4 in wellimite structure. Photoluminescence measurements of the Tb-doped Zn2SiO4 films showed two strong emission bands at 490and 545nm. The photoluminescence lifetime was 4.6ms.

  4. Representative process sampling - in practice

    DEFF Research Database (Denmark)

    Esbensen, Kim; Friis-Pedersen, Hans Henrik; Julius, Lars Petersen

    2007-01-01

    /or periodicity; different nugget effects and process variations ranging from less than one lag to full variogram lag). Variogram data analysis leads to a fundamental decomposition into 0-D sampling vs. 1-D process variances, based on the three principal variogram parameters: range, sill and nugget effect......Didactic data sets representing a range of real-world processes are used to illustrate "how to do" representative process sampling and process characterisation. The selected process data lead to diverse variogram expressions with different systematics (no range vs. important ranges; trends and...... presented cases of variography either solved the initial problems or served to understand the reasons and causes behind the specific process structures revealed in the variograms. Process Analytical Technologies (PAT) are not complete without process TOS....

  5. Profiling and Preparation of Metabolites from Pyragrel in Human Urine by Online Solid-Phase Extraction Coupled with High Performance Liquid Chromatography Tandem Mass Spectrometry Followed by a Macroporous Resin-Based Purification Approach.

    Science.gov (United States)

    Zhao, Xin; Jiang, Jingjing; Yang, Guang; Huang, Jie; Yang, Guoping; He, Guangwei; Chu, Zhaoxing; Hang, Taijun; Fan, Guorong

    2017-03-21

    Pyragrel, a new anticoagulant drug, is derived from the molecular combination of ligustrazine and ferulic acid. Pyragrel showed significant inhibitory activity against platelet aggregation induced by adenosine diphosphate (ADP), and had been approved for a phase I clinical trial by CFDA. To characterize the metabolites of Pyragrel in human urine after intravenous administration, a reliable online solid-phase extraction couple with high performance liquid chromatography tandem mass spectrometry (online SPE-HPLC-MS(n)) method was conceived and applied. Five metabolites were detected and tentatively identified, which suggested that the major metabolic pathways of Pyragrel in human were double-bond reduction, double-bond oxidation, and then followed by glucuronide conjugation. Two main metabolites were then prepared using β-glucuronide hydrolysis and macroporous resin purification approach followed by preparative high-performance liquid chromatography (PHPLC) method, with their structures confirmed on the basis of nuclear magnetic resonance (NMR) data. This study provided information for the further study of the metabolism and excretion of Pyragrel.

  6. Preparation of Two New Diasteromeric Chiral Stationary Phases Based on (+-(18-Crown-6-2,3,11,12-tetracarboxylic Acid and (R- or (S-1-(1-Naphthylethylamine and Chiral Tethering Group Effect on the Chiral Recognition

    Directory of Open Access Journals (Sweden)

    Rajalingam Agneeswari

    2016-08-01

    Full Text Available Two new diastereomeric chiral stationary phases (CSPs based on (+-(18-crown-6-2,3,11,12-tetracarboxylic acid as a chiral tethering group and a Π-basic chiral unit such as (R-1-(1-naphthylethylamine (CSP 1 or (S-1-(1-naphthylethylamine (CSP 2 were prepared. The two CSPs were applied to the enantiomeric separation of N-(3,5-dinitrobenzoyl-1-phenylalkylamines and N-(3,5-dinitrobenzoyl-α-amino acid derivatives using 20% isopropyl alcohol in hexane as a normal mobile phase. To elucidate the effect of the two chiral units on the chiral recognition, the chiral recognition abilities of the two CSPs were compared with each other and with that of a CSP (CSP 3 based on (R-1-(1-naphthylethylamine. From the chromatographic chiral recognition results, (R-1-(1-naphthylethylamine and (+−(18-crown-6-2,3,11,12-tetracarboxylic acid constituting CSP 1 were concluded to show a cooperative (“matched” effect on the chiral recognition while (S-1-(1-naphthylethylamine and (+-(18-crown-6-2,3,11,12-tetracarboxylic acid constituting CSP 2 were concluded to show an uncooperative (“mismatched” effect on the chiral recognition. From these results, it was concluded that (+-(18-crown-6-2,3,11,12-tetracarboxylic acid can be successfully used as a chiral tethering group for the preparation of new CSPs.

  7. Preparation of Two New Diasteromeric Chiral Stationary Phases Based on (+)-(18-Crown-6)-2,3,11,12-tetracarboxylic Acid and (R)- or (S)-1-(1-Naphthyl)ethylamine and Chiral Tethering Group Effect on the Chiral Recognition.

    Science.gov (United States)

    Agneeswari, Rajalingam; Sung, Ji Yeong; Jo, Eun Sol; Jeon, Hee Young; Tamilavan, Vellaiappillai; Hyun, Myung Ho

    2016-08-12

    Two new diastereomeric chiral stationary phases (CSPs) based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid as a chiral tethering group and a Π-basic chiral unit such as (R)-1-(1-naphthyl)ethylamine (CSP 1) or (S)-1-(1-naphthyl)ethylamine (CSP 2) were prepared. The two CSPs were applied to the enantiomeric separation of N-(3,5-dinitrobenzoyl)-1-phenylalkylamines and N-(3,5-dinitrobenzoyl)-α-amino acid derivatives using 20% isopropyl alcohol in hexane as a normal mobile phase. To elucidate the effect of the two chiral units on the chiral recognition, the chiral recognition abilities of the two CSPs were compared with each other and with that of a CSP (CSP 3) based on (R)-1-(1-naphthyl)ethylamine. From the chromatographic chiral recognition results, (R)-1-(1-naphthyl)ethylamine and (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid constituting CSP 1 were concluded to show a cooperative ("matched") effect on the chiral recognition while (S)-1-(1-naphthyl)ethylamine and (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid constituting CSP 2 were concluded to show an uncooperative ("mismatched") effect on the chiral recognition. From these results, it was concluded that (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid can be successfully used as a chiral tethering group for the preparation of new CSPs.

  8. New Reaction Routes for Preparing Single-Phase Tl2CaBa2Cu2O8 and Tl2Ca2Ba2Cu3O10 Powders from Stoichiometric Mixtures

    Science.gov (United States)

    Wu, Nae-Lih; Lee, Sern-Nan; Yao, Yeong Der

    1989-08-01

    Single-phase Tl2CaBa2Cu2O8 and Tl2Ca2Ba2Cu3O10 powders were prepared from stoichiometric mixtures by the following two reactions: (1) CaBa2CuO4+Tl2O3+CuO→Tl2CaBa2Cu2O8 and (2) Tl2CaBa2Cu2O8+CaO+CuO→Tl2Ca2Ba2Cu3O10. Single-phase powders were obtained at 830°C for the first reaction, and at 870°C for the second reaction. At these temperatures, the extent of powder melting and the rate of Tl loss were small. Powders thus prepared showed superconducting temperatures (both the zero-resistivity and diamagnetic onset temperatures) of above 110 K and a saturation Meissner effect of 20% of (-1/4π) at a field of 20 G.

  9. TiO{sub 2} based photo-catalysts prepared by chemical vapor infiltration (CVI) on micro-fibrous substrates; Photocatalyseurs a base de TiO{sub 2} prepares par infiltration chimique en phase vapeur (CVI) sur supports microfibreux

    Energy Technology Data Exchange (ETDEWEB)

    Sarantopoulos, Ch

    2007-10-15

    This thesis deals with micro-fibrous glass substrates functionalized with TiO{sub 2}. The oxide is deposited as a thin film onto the micro fibres by chemical vapour infiltration (CVI), yielding a photo-catalytic material usable for cleaning polluted air. We studied the relation between the structure of the material and its photo-catalytic efficiency. TiO{sub 2} thin films were prepared at low pressure, in a hot-wall CVD reactor, using Ti(O-iPr){sub 4} as a precursor. They were characterized by XRD, SEM, EDX, XPS and BET, and by recording the kinetics of decomposition of varied pollutants in solution (orange G, malic acid, imazapyr) and in air (toluene). The conditions favoring the growth of porous films through a columnar growth mode were established by MOCVD-depositing TiO{sub 2} thin films on flat substrates. The subsequent works with micro fibrous thick substrates showed the uniformity of infiltration to be the main factor governing the photo-catalytic efficiency. Operating parameters that optimize infiltration do not yield columnar growth mode. A compromise is necessary. Our photo-catalysts are showing high efficiency comparable, if not higher, to those actually commercialized. These promising results are opening real perspectives for the proposed process. (author)

  10. Magnetocaloric effect in a dual-phase coupled LaFe11Si2 crystal prepared by a modified high-pressure zone-melting technique

    Science.gov (United States)

    Feng, Shutong; Fang, Yue; Zhai, Qijie; Luo, Zhiping; Zheng, Hongxing

    2016-10-01

    A modified high-pressure optical zone-melting technique was adopted to grow a rare-earth-based LaFe11Si2 crystal in the present work. Dual-phase coupled microstructure was obtained where aligned α(Fe) phase distributed in the La(Fe,Si)13 matrix. Magnetic measurements showed that the produced crystal underwent a second-order magnetic transition in the vicinity of 250 K. Under a magnetic field change of 30 kOe, the refrigeration capacity (RC) of the produced crystal reached up to 162 J/kg. It was confirmed that zone-melting crystal growth technique is an effective approach to strikingly enhance the magnetocaloric effect of La-Fe-Si refrigeration materials.

  11. Judgments of and by Representativeness

    Science.gov (United States)

    1981-05-15

    probably agree that John Updike is a more representative American writer than Norman Mailer. rlearly, such a judgment does not have a frequentistic...example, in an early study we presented people with the following description, " John is 27 years old, with an outgoing personality. At college he was an...outstanding athlete but did not show much ability or interest in in- tellectual matters". We found that John was judged to be more likely to be "a gym

  12. The use of solid phase microextraction as sample preparation technique for determination of n-nitrosodimethylamine in water polluted by hydrazine-based rocket fuel

    Directory of Open Access Journals (Sweden)

    Bulat Kenessov

    2009-05-01

    Full Text Available A paper describes a method for determination of N-nitrosodimethylamine in water, polluted by spills of 1,1-dimethylhydrazine, based on solid phase microextraction coupled to gas chromatography/mass spectrometry. A method detection limit was determined to be 1 ug/kg, relative error was below 20%. A method is very sensitive and selective as well as quite simple, relatively cheap and fully automated.

  13. Preparation of L-Phenylalanine Chiral Stationary Phase%L-苯丙氨酸手性固定相的制备

    Institute of Scientific and Technical Information of China (English)

    章文军; 梁莉; 李慧

    2012-01-01

    L-Phenylalanine CSP was prepared from L-phenylalanine and stearoyl chloride via esterification, amidation, saponification and acid chloride reaction. The CSP was characterized by means of FTIR,1HNMR spectra and elemental analysis. Thin layer chromatography was prepared from the CSP and silica gel based on a mass ratio of 3:1. Using the development system of V(ethanol) :V (ethyl acetate):V(triethylamine) = 11:5:1 ,duloxetine was separated on the TLC,with (R)-duloxetine Rf1 =0. 87, (S) -duloxetine Rf2 =0. 75.%L-苯丙氨酸和硬酯酰氯经酯化、酰胺化、皂化和酰氯化反应得到新型手性固定相,用FTIR、1HNMR和元素分析对手性固定相(CSP)进行了表征.将制得的手性固定相按m(CSP)∶m(硅胶)=3∶1制备薄层色谱板,采用V(乙醇)∶V(乙酸乙酯)∶V(三乙胺)=11∶5∶1作为展开体系,对手性药物度洛西汀进行拆分,其中右旋度洛西汀Rf =0.87,左旋度洛西汀Rf2 =0.75.

  14. Phase Vocoder

    Directory of Open Access Journals (Sweden)

    J.L. Flanagan

    2013-08-01

    Full Text Available A vocoder technique is described in which speech signals are represented by their short-time phase and amplitude spectra. A complete transmission system utilizing this approach is simulated on a digital computer. The encoding method leads to an economy in transmission bandwidth and to a means for time compression and expansion of speech signals.

  15. Preparation of CdS Nanoparticles in Aqueous Phase and Photocatalytic Degradation of Rhodamine B%硫化镉纳米粒子的水相制备及光催化降解罗丹明B

    Institute of Scientific and Technical Information of China (English)

    黄正喜; 杜锴; 胡振龙

    2012-01-01

    CdS nanoparticles were successfully prepared by a precipitation method in aqueous phase,cadmium chloride and thiosemicarbazide were used as cadmium and sulfur sources respectively.The CdS nanoparticles were characterized by X-ray diffraction(XRD),X-ray photoelectron spectroscopy(XPS),scanning electron microscope(SEM),transmission electron microscope(TEM) and UV-Vis spectrum.The photocatalytic degradation of Rhodamine B(RhB) under visible light was used as probe reactions to evaluate the photocatalytic activities of the prepared nanopartiles.The results indicated that the preparation method is simple,and the products have high photocatalytic activity.%以氯化镉为镉源,硫代氨基脲为硫源,在水相中通过沉淀法制备出硫化镉纳米颗粒,并对其进行表征.以光催化降解罗丹明B作为探针反应,评价其光催化降解活性.结果表明:该制备方法简单易行,所得纳米粒子具有良好的光催化活性.

  16. EPDM基吸油树脂型相变储能材料的制备与性能%Preparation and Property of Oil-absorbing Resin Based on EPDM as Phase Change Materials

    Institute of Scientific and Technical Information of China (English)

    周晓明

    2012-01-01

    The oil-absorbing resin based on EPDM rubber was used as a carrier for adsorption of phase change material such as paraffin to prepare solid-solid phase change materials (PCM). Suspension polymerization was adopted to develop a high oil-absorbing resin of EPDM series. SEM was used to observe the morphology before and after absorbing paraffin oil; DSC was employed to measure the phase change temperature and enthalpy after adsorbing phase change material paraffin. The results showed that the maximum adsorption capacity of paraffin on oil-absorbing resin could up to 4.9 g/g, and the phase transition enthalpy was 124. 5 J/g. It can be considered as promising PCMs.%以三元乙丙橡胶( EPDM)基吸油树脂作为载体,通过吸附石蜡作为相变物质,制备了高分子固-固相变 储能材料.采用悬浮聚合法,探讨了EPDM基高吸油树脂的合成工艺对树脂吸附石蜡性能的影响;用扫描电子显微镜观察了吸油树脂吸附石蜡前后的微观形态变化;利用差示扫描量热仪(DSC)测定了吸附相变材料后,吸油树脂的相变温度和相变焓.结果表明:EPDM基吸油树脂对石蜡的最大吸附量可达4.9 g/g,其相变焓为124.5 J/g,具有较高的应用潜力.

  17. 月桂酸-膨胀石墨复合相变材料的制备及性能%Preparation and performance of lauric acid-expanded graphite composite phase change materials

    Institute of Scientific and Technical Information of China (English)

    黄雪; 崔英德; 尹国强; 冯光炷; 吴梓敏

    2015-01-01

    The lauric acid-expanded graphite (LA/EG) composite phase change materials was prepared by using adsorption properties of porous graphite with lauric acid as phase change material, porous expanded graphite(EG) as the skeleton carrier; and through the experiment of the basic properties of shape stabilized phase change material, surface morphology, durability were studied. The results showed that lauric acid was effectively encapsulated within the pores of the expanded graphite; phase change temperature and latent heat of LA/EG was 45.45℃and 125.30 J·g?1 respectively whenmLA:mEG=95:5. LA/EG loss rate was very small after 100 times of hot and cold cycle phase transitions, which indicated that LA/EG has good stability in practice.%以月桂酸为相变材料,多孔石墨为骨架基体,利用多孔石墨的物理吸附特性,制备月桂酸-膨胀石墨定形复合相变材料.并通过实验对定形复合相变材料的基本性能、表面形貌及耐久性进行了研究.结果表明,月桂酸被有效地包封在膨胀石墨的孔隙内;m 月桂酸:m 膨胀石墨=95:5时定形复合相变材料的相变温度45.45℃,相变潜热125.30 J·g?1;经100次冷热相变循环后,复合相变材料损失量非常少,表明月桂酸-膨胀石墨复合相变材料在实践中有良好的稳定性.

  18. Preparation and research on heat preservation performance of porous phase change energy storage granule material%多孔相变储能颗粒的制备及蓄热性能研究

    Institute of Scientific and Technical Information of China (English)

    李书进; 蒋晓曙; 刘燕; 厉见芬

    2012-01-01

    In this article,with lauric -capric acid composite as PCM, expanded perlite, expanded vermiculite and expanded graphite three porous particles as enclosed carrier, three kinds of phase change energy storage granule were prepared by vacuum adsorption and melt impregnation method. Morphology of porous particles before and after the adsorption of PCM was observed through SEM. Phase change temperature and latent heat of energy storage granule were tested by TG-DSC. The results showed that, three kinds of phase change energy storage granule all fall in human comfort temperature range; PCM adsorption quantity and microstructure of porous particle exists direct correlation; after 150 times thermal cycles, phase change temperature and latent heat of phase change energy storage granule were stable.%以月桂酸-癸酸复合二元酸作为PCM,以膨胀珍珠岩、膨胀蛭石和膨胀石墨3种多孔颗粒作为封装载体,用真空吸附-熔融浸渍法制备了3种多孔相变储能颗粒.通过SEM观测多孔颗粒吸附PCM前后的形貌,并用TG-DSC测试多孔相变储能颗粒的相变温度和相变潜热.结果表明,3种多孔相变储能颗粒的相变温度均在人体舒适度范围内;多孔颗粒的微观结构与PCM吸附量存在直接关系;经受150次冷热循环后,多孔相变储能颗粒的相变温度和相变潜热均比较稳定.

  19. Phase Composition of Ni/Mg1−xNixO as a Catalyst Prepared for Selective Methanation of CO in H2-Rich Gas

    OpenAIRE

    Mengmeng Zhang; Hongwei Ma; Zhiming Gao

    2015-01-01

    Supported Ni catalysts Ni/Mg1−xNixO were prepared by reducing samples NiO-MgO in H2/N2 mixture gas at 500°C~800°C for selective methanation of CO in H2-rich gas (CO-SMET). The samples NiO-MgO were obtained by heating water slurry of MgO and Ni(NO3)2 in a rotary evaporator at 80°C and a final calcination in air at 400°C~800°C. X-ray diffraction (XRD) and temperature programmed reduction (TPR) measurements demonstrate that the samples NiO-MgO were composed of solid solution Mg1−yNiyO as the mai...

  20. 谈项目施工准备阶段的技术管理%On technical management at construction preparation phase of projects

    Institute of Scientific and Technical Information of China (English)

    杜晋刚

    2016-01-01

    Combining with the work experience,the paper illustrates the technical management measures at the program construction preparation from the familiarity with contracts,map checking,progress planning,special construction scheme compilation,and technical rechecking,so as to improve the economic benefits with the technical measures and realize the cost target.%结合工作经验,从熟悉合同、查看图纸、进度计划、专项施工方案编制、技术复核等方面,阐述了项目施工准备阶段的技术管理措施,旨在通过技术手段提高经济效益,从而实现目标成本。

  1. Representing culture in interstellar messages

    Science.gov (United States)

    Vakoch, Douglas A.

    2008-09-01

    As scholars involved with the Search for Extraterrestrial Intelligence (SETI) have contemplated how we might portray humankind in any messages sent to civilizations beyond Earth, one of the challenges they face is adequately representing the diversity of human cultures. For example, in a 2003 workshop in Paris sponsored by the SETI Institute, the International Academy of Astronautics (IAA) SETI Permanent Study Group, the International Society for the Arts, Sciences and Technology (ISAST), and the John Templeton Foundation, a varied group of artists, scientists, and scholars from the humanities considered how to encode notions of altruism in interstellar messages art_science/2003>. Though the group represented 10 countries, most were from Europe and North America, leading to the group's recommendation that subsequent discussions on the topic should include more globally representative perspectives. As a result, the IAA Study Group on Interstellar Message Construction and the SETI Institute sponsored a follow-up workshop in Santa Fe, New Mexico, USA in February 2005. The Santa Fe workshop brought together scholars from a range of disciplines including anthropology, archaeology, chemistry, communication science, philosophy, and psychology. Participants included scholars familiar with interstellar message design as well as specialists in cross-cultural research who had participated in the Symposium on Altruism in Cross-cultural Perspective, held just prior to the workshop during the annual conference of the Society for Cross-cultural Research . The workshop included discussion of how cultural understandings of altruism can complement and critique the more biologically based models of altruism proposed for interstellar messages at the 2003 Paris workshop. This paper, written by the chair of both the Paris and Santa Fe workshops, will explore the challenges of communicating concepts of altruism that draw on both biological and cultural models.

  2. Phase Composition Control of Calcium Phosphate Nanoparticles for Tunable Drug Delivery Kinetics and Treatment of Osteomyelitis. Part 1: Preparation and Drug Release

    Science.gov (United States)

    Uskoković, Vuk; Desai, Tejal A.

    2012-01-01

    Developed in this study is a multifunctional material for simultaneous osseoinduction and drug delivery, potentially applicable in the treatment of osteomyelitis. It is composed of agglomerates of nanoparticles of calcium phosphate (CAP) with different monophasic contents. The drug loading capacity and the release kinetics were investigated on two model drug compounds with different chemical structures, sizes and adsorption propensities: bovine serum albumin and fluorescein. Loading of CAP powders with small molecule drugs was achieved by physisorption and desiccation-induced agglomeration of nanoparticulate subunits into microscopic blocks. The material dissolution rate and the drug release rate depended on the nature of the CAP phase, decreasing from monocalcium phosphate to monetite to amorphous CAP and calcium pyrophosphate to hydroxyapatite. The sustained release of the two model drugs was shown to be directly relatable to the degradation rate of CAP carriers. It was demonstrated that the degradation rate of the carrier and the drug release kinetics could be made tunable within the time scale of 1–2 h for the most soluble CAP phase, monocalcium phosphate, to 1–2 years for the least soluble one, hydroxyapatite. From the standpoint of antibiotic therapy for osteomyelitis, typically lasting for six weeks, the most prospective CAP powder was amorphous CAP with its release time scale for a small organic molecule, the same category to which antibiotics belong, of 1 – 2 months under the conditions applied in our experiments. By combining these different CAP phases in various proportions, drug release profiles could be tailored to the therapeutic occasion. PMID:23115118

  3. Semantic Representatives of the Concept

    Directory of Open Access Journals (Sweden)

    Elena N. Tsay

    2013-01-01

    Full Text Available In the article concept as one of the principle notions of cognitive linguistics is investigated. Considering concept as culture phenomenon, having language realization and ethnocultural peculiarities, the description of the concept “happiness” is presented. Lexical and semantic paradigm of the concept of happiness correlates with a great number of lexical and semantic variants. In the work semantic representatives of the concept of happiness, covering supreme spiritual values are revealed and semantic interpretation of their functioning in the Biblical discourse is given.

  4. Single column comprehensive analysis of pharmaceutical preparations using dual-injection mixed-mode (ion-exchange and reversed-phase) and hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Kazarian, Artaches A; Taylor, Mark R; Haddad, Paul R; Nesterenko, Pavel N; Paull, Brett

    2013-12-01

    The comprehensive separation and detection of hydrophobic and hydrophilic active pharmaceutical ingredients (APIs), their counter-ions (organic, inorganic) and excipients, using a single mixed-mode chromatographic column, and a dual injection approach is presented. Using a mixed-mode Thermo Fisher Acclaim Trinity P1 column, APIs, their counter-ions and possible degradants were first separated using a combination of anion-exchange, cation-exchange and hydrophobic interactions, using a mobile phase consisting of a dual organic modifier/salt concentration gradient. A complementary method was also developed using the same column for the separation of hydrophilic bulk excipients, using hydrophilic interaction liquid chromatography (HILIC) under high organic solvent mobile phase conditions. These two methods were then combined within a single gradient run using dual sample injection, with the first injection at the start of the applied gradient (mixed-mode retention of solutes), followed by a second sample injection at the end of the gradient (HILIC retention of solutes). Detection using both ultraviolet absorbance and refractive index enabled the sensitive detection of APIs and UV-absorbing counter-ions, together with quantitative determination of bulk excipients. The developed approach was applied successfully to the analysis of a dry powder inhalers (Flixotide(®), Spiriva(®)), enabling comprehensive quantification of all APIs and excipients in the sample.

  5. Preparation of molecular imprinted microspheres based on inorganic-organic co-functional monomer for miniaturized solid-phase extraction of fluoroquinolones in milk.

    Science.gov (United States)

    Wang, Hui; Wang, Ruiling; Han, Yehong

    2014-02-15

    An inorganic-organic co-functional monomer, methacrylic acid-vinyltriethoxysilan (MAA-VTES) was designed for the synthesis of molecularly imprinted microspheres (MIMs). By virtue of the aqueous suspension polymerization and dummy template (pazufloxacin), the obtained MAA-VTES based MIMs exhibited good recognition and selectivity to fluoroquinolones (FQs), and were successfully applied as selective sorbents of a miniaturized home-made solid phase extraction device for the determination of ofloxacin (OFL), lomefloxacin (LOM) and ciprofloxacin (CIP) in milk samples. Under the optimum conditions of the miniaturized molecularly imprinted solid phase extraction (mini-MISPE) coupled with liquid chromatography-ultraviolet detector (LC-UV), good linearities were obtained for three FQs in a range of 0.2-20.0μgmL(-1) and the average recoveries at three spiked levels were ranged from 87.2% to 106.1% with the relative standard deviation (RSD) less than 5.4%. The presented co-functional monomer based mini-MISPE-LC-UV protocol introduced the rigidity and flexibility of inorganic silicon materials, exhibited excellent extraction performance towards targets, and could be potentially applied to the determination of FQs in milk samples.

  6. Preparation and investigations of thermal properties of copper oxide, aluminium oxide and graphite based on new organic phase change material for thermal energy storage

    Indian Academy of Sciences (India)

    Murat Genc; Betul Inci; Zuhal Karagoz Genc; Canan Aksu Canbay; Memet Sekercı

    2015-04-01

    The effects of copper oxide, aluminium oxide and graphite on the thermal and structural properties of the organic phase change material (PCM) were investigated. Ethyl 2-(1H-benzotriazole-1-yl)acetate was selected as the pure PCM. Fourier transform infrared (FT-IR) spectroscopy, X-ray, energy dispersive X-ray (EDX) and scanning electron microscope (SEM) were used to determine the chemical structure, crystalloid phase, chemical composition and microstructure of the composites, respectively. The thermal properties were investigated by differential scanning calorimetry and thermogravimetric analyzer. The FT-IR analyses indicated that there was no chemical interaction between the pure PCM and the supporting materials such as copper oxide, aluminium oxide and graphite. The X-ray diffractograms of the samples were nearly the same, but the peak intensities changed according to the supporting materials. The SEM results showed that the C, N and O elements were well adsorbed into the porous network of the graphite, Al2O3 and CuO. According to the supporting materials, the graphite had the minimum porosity and the maximum crystallite size.

  7. Development and validation of a reversed-phase ion-pair high-performance liquid chromatographic method for the determination of risedronate in pharmaceutical preparations.

    Science.gov (United States)

    Kyriakides, Demetra; Panderi, Irene

    2007-02-12

    A stability indicating, reversed-phase ion-pair high-performance liquid chromatographic method was developed and validated for the determination of risedronate in pharmaceutical dosage forms. The determination was performed on a BDS C(18) analytical column (250 mm x 4.6 mm i.d., 5 microm particle size); the mobile phase consisted of 0.005 M tetrabutylammonium hydroxide and 0.005 M pyrophosphate sodium (pH 7.0) mixed with acetonitrile in a ratio (78:22, v/v) and pumped at a flow rate 1.00 mL min(-1). The ultraviolet (UV) detector was operated at 262 nm. The retention times of magnesium ascorbyl phosphate, which was used as internal standard and risedronate were 4.94 and 5.95 min, respectively. The calibration graph was ranged from 2.50 to 20.00 microg mL(-1), while detection and quantitation limits were found to be 0.48 and 1.61 microg mL(-1), respectively. The intra- and inter-day percentage relative standard deviations, %R.S.D., were less than 5.9%, while the relative percentage error, %E(r), was less than 0.4%. The method was applied to the quality control of commercial tablets and content uniformity test and proved to be suitable for rapid and reliable quality control.

  8. Reversed-phase vortex-assisted liquid-liquid microextraction: a new sample preparation method for the determination of amygdalin in oil and kernel samples.

    Science.gov (United States)

    Hosseini, Mohammad; Heydari, Rouhollah; Alimoradi, Mohammad

    2015-02-01

    A novel, simple, and rapid reversed-phase vortex-assisted liquid-liquid microextraction coupled with high-performance liquid chromatography has been introduced for the extraction, clean-up, and preconcentration of amygdalin in oil and kernel samples. In this technique, deionized water was used as the extracting solvent. Unlike the reversed-phase dispersive liquid-liquid microextraction, dispersive solvent was eliminated in the proposed method. Various parameters that affected the extraction efficiency, such as extracting solvent volume and its pH, vortex, and centrifuging times were evaluated and optimized. The calibration curve shows good linearity (r(2) = 0.9955) and precision (RSD < 5.2%) in the range of 0.07-20 μg/mL. The limit of detection and limit of quantitation were 0.02 and 0.07 μg/mL, respectively. The recoveries were in the range of 96.0-102.0% with relative standard deviation values ranging from 4.0 to 5.1%. Unlike the conventional extraction methods for plant extracts, no evaporative and re-solubilizing operations were needed in the proposed technique. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Representative mass reduction in sampling

    DEFF Research Database (Denmark)

    Petersen, Lars; Esbensen, Harry Kim; Dahl, Casper Kierulf

    2004-01-01

    We here present a comprehensive survey of current mass reduction principles and hardware available in the current market. We conduct a rigorous comparison study of the performance of 17 field and/or laboratory instruments or methods which are quantitatively characterized (and ranked) for accuracy...... always be representative in the full Theory of Sampling (TOS) sense. This survey also allows empirical verification of the merits of the famous ??Gy?s formula?? for order-of-magnitude estimation of the Fundamental Sampling Error (FSE).......We here present a comprehensive survey of current mass reduction principles and hardware available in the current market. We conduct a rigorous comparison study of the performance of 17 field and/or laboratory instruments or methods which are quantitatively characterized (and ranked) for accuracy...... dividers, the Boerner Divider, the ??spoon method??, alternate/fractional shoveling and grab sampling. Only devices based on riffle splitting principles (static or rotational) passes the ultimate representativity test (with minor, but significant relative differences). Grab sampling, the overwhelmingly...

  10. In situ-Raman studies on thermally induced structural changes of porous MoO{sub 3} prepared in vapor phase under He and H{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Diaz-Droguett, D.E., E-mail: dodiaz@fis.puc.cl [Departamento de Fisica, Facultad de Fisica, Pontificia Universidad Catolica de Chile, Santiago (Chile); El Far, R. [Departamento de Fisica, Facultad de Fisica, Pontificia Universidad Catolica de Chile, Santiago (Chile); Fuenzalida, V.M. [Departamento de Fisica, Facultad de Ciencias Fisicas y Matematicas, Universidad de Chile, Santiago (Chile); Cabrera, A.L. [Departamento de Fisica, Facultad de Fisica, Pontificia Universidad Catolica de Chile, Santiago (Chile)

    2012-06-15

    The structural transformations induced by heating on MoO{sub 3} mesoporous samples grown in vapor-phase under helium and hydrogen were studied by in situ Raman spectroscopy. The samples were continuously irradiated by a He-Ne laser of 5.5 mW for 105 min and Raman spectra were dynamically acquired every 5 min, in order to evaluate the laser effects. The He-grown sample did not undergo structural transformations due to the laser irradiation while the H{sub 2}-grown sample underwent changes after just 10 min of irradiation. On the other hand, each type of sample was heated in air from room temperature up to 450 Degree-Sign C using a heating rate of 5 Degree-Sign C min{sup -1} and Raman spectra were recorded each 25 Degree-Sign C. The He-grown sample remained structural unchanged up to 250 Degree-Sign C revealing a high temperature state of its amorphous matrix whereas the H{sub 2}-grown sample exhibited changes around 70 Degree-Sign C. These changes were attributed to the crystallization onset of its amorphous matrix to {beta}-MoO{sub 3}. However, this same transition was detected between 250 Degree-Sign C and 275 Degree-Sign C for the He-grown sample. A second transformation was detected in both samples in a temperature range more similar associated to the transition of the formed {beta}-MoO{sub 3} phase to {alpha}-MoO{sub 3}. After the heat treatment, the oxide of both samples was slightly reduced, as revealed by XPS analysis. The metastability at low temperatures of the amorphous phase of the H{sub 2}-grown sample could be associated to release of hydrogen trapped inside the compound and to the break of weak bonds between Mo and OH groups. At high temperatures, above 225 Degree-Sign C, the rapid conversion to {beta}-MoO{sub 3} of the amorphous matrix of the H{sub 2}-grown sample occurred due to the dehydration of the sample. - Highlights: Black-Right-Pointing-Pointer Porous MoO{sub 3} grown in He or H{sub 2} showed structural differences by heating effects. Black

  11. Microstructure of MgB{sub 2} superconducting wire prepared by internal magnesium diffusion and in-situ powder-in-tube processes – Secondary phase intergrain nanolayers as an oxygen content indicator

    Energy Technology Data Exchange (ETDEWEB)

    Rosová, A., E-mail: alica.rosova@savba.sk; Kováč, P.; Hušek, I.; Brunner, B.; Dobročka, E.

    2015-09-15

    Highlights: • We compared microstructure of undoped MgB{sub 2} wires made by in-situ PIT and IMD. • The main differences were in MgB{sub 2} density and volume ratio of amorphous MgO. • Thin oriented layers of secondary phases were observed between MgB{sub 2} plate grains. • Only MgO or only Mg oriented layers were in the PIT or IMD samples, resp. • High MgB{sub 2} density and low MgO{sub 2} content caused higher J{sub c} of IMD wire. - Abstract: We analyzed microstructure of two undoped MgB{sub 2} single core wires prepared by two different technologies – in-situ powder-in-tube (PIT) technology and internal magnesium diffusion (IMD) processes. Their microstructure showed mainly different densities of superconducting material, corresponding content of pores and the volume ratio of amorphous MgO phase. We observed a special microstructural feature – thin oriented secondary phase layers on grain boundaries of plate-shaped MgB{sub 2} grains. The significant decrease of oxygen content in IMD wire was reflected in the presence of thin oriented Mg layers while in PIT wire thin oriented MgO layers were observed. The microstructure difference is reflected in increased critical current density J{sub c} of the IMD wire in comparison to the PIT one.

  12. Preparation of a novel ionic hybrid stationary phase by non-covalent functionalization of single-walled carbon nanotubes with amino-derivatized silica gel for fast HPLC separation of aromatic compounds.

    Science.gov (United States)

    Aral, Hayriye; Çelik, K Serdar; Aral, Tarık; Topal, Giray

    2016-03-01

    Single-walled carbon nanotubes (SWCNTs) were immobilized on spherical silica gel with a 4-μm average particle size and a 60-Å average pore size. The amino-derivatized silica gel was non-covalently coated with carboxylated SWCNTs to preserve the structure of the nanotubes and their physico-chemical properties. The novel ionic hybrid stationary phase was characterized by scanning electron microscopy (SEM), infra-red (IR) spectroscopy and elemental analysis, and then, it was used to fill an empty 150×4.6mm(2) high-performance liquid chromatography (HPLC) column. Chromatographic parameters, such as the theoretical plate number, retention factor and peak asymmetry factor, and analytical parameters, such as the limit of detection (LOD), limit of quantification (LOQ), linear range, calibration equation, and R(2) value, and quantitative analysis parameters were calculated for all of the analytes. Using different mobile phases, five different classes of aromatic hydrocarbons were separated in a very short analysis time of 4-8min. Furthermore, a high theoretical plate number (up to 25000) and an excellent peak asymmetry factor (1.0) were obtained. The results showed that the surface of the SWNTs had very strong interactions with aromatic groups, therefore providing high selectivity for the separation of different classes of aromatic compounds. This study indicates that SWCNTs enable the extension of the application range of the newly prepared stationary phases for the fast separation of aromatic compounds by HPLC.

  13. Sample Preparation for Bioanalytical and Pharmaceutical Analysis.

    Science.gov (United States)

    Clark, Kevin D; Zhang, Cheng; Anderson, Jared L

    2016-12-06

    Biological and pharmaceutical samples represent formidable challenges in sample preparation that hold important consequences for bioanalysis and genotoxic impurity quantification. This Feature will emphasize significant advances toward the development of rapid, sensitive, and selective sample preparation methods.

  14. Growth and characteristics of InAsSb epilayers with a cutoff wavelength of 4.8 μm prepared by one-step liquid phase epitaxy

    Institute of Scientific and Technical Information of China (English)

    GAO Yuzhu; GONG Xiuying; FANG Weizheng; Akiniro Ishida

    2009-01-01

    InAsSb epilayers with a cutoff wavelength of 4.8 μm have been successfully grown on InAs substrates by one-step liquid phase epitaxy (LPE) technology. The epilayers were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) transmittance measurements and scanning electron microscopy (SEM). The influence of different growth conditions on the optical and structural properties of the materi-als was studied. The results revealed that the good crystalline quality, mirror smooth surface and flat interface of InAsSb epilayers were achieved. They benefited from optimized growth conditions, i.e., sufficient homogeneity of the growth melt and a very slow cooling rate.

  15. Representing Conversations for Scalable Overhearing

    CERN Document Server

    Gutnik, G; 10.1613/jair.1829

    2011-01-01

    Open distributed multi-agent systems are gaining interest in the academic community and in industry. In such open settings, agents are often coordinated using standardized agent conversation protocols. The representation of such protocols (for analysis, validation, monitoring, etc) is an important aspect of multi-agent applications. Recently, Petri nets have been shown to be an interesting approach to such representation, and radically different approaches using Petri nets have been proposed. However, their relative strengths and weaknesses have not been examined. Moreover, their scalability and suitability for different tasks have not been addressed. This paper addresses both these challenges. First, we analyze existing Petri net representations in terms of their scalability and appropriateness for overhearing, an important task in monitoring open multi-agent systems. Then, building on the insights gained, we introduce a novel representation using Colored Petri nets that explicitly represent legal joint conv...

  16. [Preparation of an agglomerated ion chromatographic stationary phase with 2,3-ionene and its application in SO4(2-) analysis].

    Science.gov (United States)

    Wang, Muhua; Liu, Junwei; Huang, Zhongping; Zhang, Jiajie; Zhu, Yan

    2015-07-01

    The poly-electrolyte cation functional group of 2,3-ionene was synthesized with tetramethyl ethylenediamine and 1,3-dibromopropane as the raw materials. Multiporous polystyrene-divinylbenzene microsphere particles (PS-DVB) were produced by swelling method with polystyrene as seeds and sulfonated. Then the 2,3-ionene was bonded on the sulfonated multi-porous polystyrene-divinylbenzene microsphere particles by agglomeration to get the agglomerative ion-exchange stationary phase. After optimizing the synthetic conditions, the new stationary phase was characterized by the techniques including scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and elemental analysis. The chromatographic column was packed by slurry method and applied in the analysis of SO4(2-) with a conductivity detector. SO4(2-) and other six common anions including F-, Cl-, NO2(-), Br-, NO3(-), PO4(3-), were separated and analyzed rapidly on the self-regulating chromatographic column within 8 min. The linear range was from 0.5 to 50 mg/L with correlation coefficient (r) of 0.9992. The LOD was 0.04 mg/L with S/N of 3. The relative standard deviations (RSDs, n = 6) were 2.4% and 3.1% for the peak area and retention time, respectively. The recoveries were between 99.2% and 101.8%. The retention times of SO4(2-) did not change significantly after long time use of the self-regulating chromatographic column. The self-regulating chromatographic column is suitable for the detection of SO4(2-) in complex matrix samples.

  17. Preparation of anisotropic magnetic FeNiPt2 films on MgO(001): Atomistic mechanisms for the interdiffusion of two L10 phases

    Science.gov (United States)

    Montsouka, R. V. P.; Goyhenex, C.; Schmerber, G.; Ulhaq-Bouillet, C.; Derory, A.; Faerber, J.; Arabski, J.; Pierron-Bohnes, V.

    2006-10-01

    L10 -ordered FeNiPt2(001) thin films were prepared by the interdiffusion of FePt(001) and NiPt(001) layers codeposited on MgO(001) substrates by molecular beam epitaxy (MBE). A large uniaxial magnetic anisotropy (Ku=9.105J/m3) and a reduced magnetic transition temperature (Tc=400K) were obtained. Growth at 700K and a first annealing at 800K result in a large long-range order parameter reflecting the concentration modulation along the growth direction. This high long-range order parameter is conserved in the FeNiPt2 layers after interdiffusion at 900K , contrary to what is expected from a simple vacancy migration process. This experimental observation can be explained either by a 6-jump cycle mechanism or by the alternate diffusion of a double vacancy, which are both favored energetically over a second-nearest-neighbor jump mechanism or the simultaneous diffusion of a double vacancy as shown by quenched molecular dynamics simulations.

  18. Preparation and activity evaluation of NiMoB/γ-Al2O3 catalyst by liquid-phase furfural hydrogenation

    Institute of Scientific and Technical Information of China (English)

    Shuqin Wei; Hongyou Cui; Jinghua Wang; Shuping Zhuo; Weiming Yi; Lihong Wang; Zhihe Li

    2011-01-01

    Amorphous MoNiB/γ-Al2O3 alloy catalysts were prepared by reducing NiCl2-6H2O and genation of furfural (FFR) as a probe reaction,the activity of MoNiB/γ-Al2O3 was examined. Compared to NiB and NiMoB,NiMoB/γ-Al2O3 exhibited excellent activity and selectivity towards furfuryl alcohol (FFA). After reaction for 3.0 h at 80 °C and 5.0 MPa in methanol,FFR conversion reached 99% with FFA yield of 91%. The effects of doping amount of Mo and calcination temperature before NaBH4 reduction on hydrogenation activity were also investigated. The optimum Mo/Ni atom ratio and calcination temperature were found to be 1:7 and 300 C,respectively. XRD patterns and SEM images indicated that NiMoB over the surface of γ-Al2O3 was amorphous and highly dispersed,which was responsible for the high thermal stability of the title catalyst.

  19. Preparation, thermal and flammability properties of a novel form-stable phase change materials based on high density polyethylene/poly(ethylene-co-vinyl acetate)/organophilic montmorillonite nanocomposites/paraffin compounds

    Energy Technology Data Exchange (ETDEWEB)

    Cai, Yibing [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, Anhui 230027 (China); Key Laboratory of Eco-textiles, Ministry of Education, Jiangnan University, Wuxi, Jiangsu 214122 (China); Song, Lei; He, Qingliang; Yang, Dandan; Hu, Yuan [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, Anhui 230027 (China)

    2008-08-15

    The paraffin is one of important thermal energy storage materials with many desirable characteristics (i.e., high heat of fusion, varied phase change temperature, negligible supercooling, self-nucleating, no phase segregation and cheap, etc.), but has low thermal stability and flammable. Hence, a novel form-stable phase change materials (PCM) based on high density polyethylene (HDPE)/poly(ethylene-co-vinyl acetate) (EVA)/organophilic montmorillonite (OMT) nanocomposites and paraffin are prepared by twin-screw extruder technique. The structures of the HDPE-EVA/OMT nanocomposites and the form-stable PCM are evidenced by the X-ray diffraction (XRD), transmission electronic microscopy (TEM) and scanning electronic microscope (SEM). The results of XRD and TEM show that the HDPE-EVA/OMT nanocomposites form the ordered intercalated nanomorphology. The form-stable PCM consists of the paraffin, which acts as a dispersed phase change material and the HDPE-EVA/OMT nanocomposites, which acts as the supporting material. The paraffin disperses in the three-dimensional net structure formed by HDPE-EVA/OMT nanocomposites. The thermal stability, latent heat and flammability properties are characterized by thermogravimetry analysis (TGA), dynamic Fourier-transform infrared (FTIR), differential scanning calorimeter (DSC) and cone calorimeter, respectively. The TGA and dynamic FTIR analyses indicate that the inc